WO2023211862A1 - Rapid, low cost, volatile accumulation sensing instrument for rancidity measurement in nuts and oils - Google Patents

Rapid, low cost, volatile accumulation sensing instrument for rancidity measurement in nuts and oils Download PDF

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Publication number
WO2023211862A1
WO2023211862A1 PCT/US2023/019670 US2023019670W WO2023211862A1 WO 2023211862 A1 WO2023211862 A1 WO 2023211862A1 US 2023019670 W US2023019670 W US 2023019670W WO 2023211862 A1 WO2023211862 A1 WO 2023211862A1
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volatile organic
sample
organic compounds
container
sensors
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PCT/US2023/019670
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French (fr)
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Elizabeth J. MITCHAM
Nicholas F. REITZ
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The Regents Of The University Of California
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Publication of WO2023211862A1 publication Critical patent/WO2023211862A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/02Food
    • G01N33/03Edible oils or edible fats

Definitions

  • This technology pertains generally to systems and methods for the detection and quantification of spoilage or rancidity in foods and more particularly to inexpensive devices and methods for quickly measuring volatile organic compounds and the rate of change of accumulation as an assessment of spoilage.
  • samples of perishable foods may be analyzed by techniques such as spectrophotometric assays, chromatographic assays, immunoassays and bacterial activity assays to determine spoilage.
  • the analysis of foods for contaminants or degradation products as an indicator of spoilage can be a complex task typically producing a time delay between the sampling and the receipt of results. During this delay, the content of indicators and the degree of spoilage may change leading to an erroneous assessment of spoilage or rancidity. In many instances, repeated sampling or continuous sampling and testing of a commodity is desirable to monitor daily changes or the rate of spoilage. Therefore, testing procedures that are accurate, quick and non-destructive are essential.
  • lipid oxidation is a significant contributor to food spoilage in high lipid content foods, such as nuts, seeds, and oils. Lipid oxidation is commonly measured throughout the food industry as a measure of spoilage.
  • common oxidation measurements including peroxide value, require high labor inputs, hazardous chemicals, and dedicated lab space.
  • Current methods for lipid oxidation measurements include hexanal and peroxide value determination. While both are used regularly, each has drawbacks that can make obtaining results difficult, expensive, time consuming and unreliable.
  • hexanal is a breakdown product of lipid oxidation that is typically measured using gas chromatography.
  • Gas chromatography measurement of hexanal is reproducible and proportional to total lipid oxidation for most products but requires expensive (>$10,000) equipment and costly consumables as well as technically competent personnel. Additionally, the sample is often heated to release the volatiles, making gas chromatography a destructive method.
  • a typical hexanal chromatography analysis of a sample typically requires about 45 minutes to run.
  • a peroxide value is determined by well-established methods involving titration. Peroxide value measurements do not require specialized or expensive equipment. However, the process does involve significant chemical and labor inputs. A typical peroxide value determination by titration requires approximately 15 minutes per sample to run, produces hazardous chemical wastes, and is also a destructive method.
  • the largest disadvantage of the titration method for peroxide value determination is that it measures an intermediary product of oxidation rather than its chemical or labor requirements. As lipids oxidize, peroxide values increase as the amount of the intermediary compound increases, but then decreases as the intermediary compound further degrades. This process can cause erroneous data and conclusions in more extensively oxidized samples.
  • a rapid, non-destructive, inexpensive system and method are provided that may be used for determining the oxidation of nuts, seeds, oils, and other lipid rich products as well as spoilage of other food products by microorganisms.
  • This portable system can be used in warehouses, packing plants, and laboratories as an indicator of lipid oxidation and other types of spoilage.
  • the system enables periodic or continuous monitoring of lipid oxidation during storage and rapid screening of perishable commodities upon receiving a shipment.
  • the system and methods measure the rate of production or accumulation of organic volatiles (TVOC) from stored lipid containing products to measure lipid oxidation and other types of spoilage.
  • TVOC organic volatiles
  • the TVOC system and methods of the technology use no consumables, is nondestructive, and takes about 1 minute to about 5 minutes per sample with no sample preparation requirements.
  • the portable system enables lipid oxidation measurements in the storage facility and no lab, chemicals, or specialized knowledge are required.
  • the equipment cost is approximately $120 for a portable system with data logging capacity, user interface, and battery. Preliminary results indicate accurate tracking of lipid oxidation trends in walnuts and olive oil. Validation is recommended for new product applications.
  • an apparatus for measuring lipid oxidation in a sample has a sample container with sensors configured to measure total volatile organic compounds (TVOC) or one or more component volatile organic compounds in the enclosed interior of the container.
  • the container preferably has a fan for agitating the atmosphere within the interior of the container to improve the accuracy of the sensors.
  • the signals from the sensors are received and processed by a computer/ controller with software for sensing the quantity or concentration of volatile organic compounds and measuring rate of accumulation of total volatile organic compounds in the enclosed interior assessing lipid oxidation and the degree of spoilage of the sample.
  • the container includes a display for displaying the quantity and measured rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors as well as displaying the assessed lipid oxidation and degree of spoilage.
  • the computer is located remotely from the container and the sensor signals are transmitted from the container to the computer for processing.
  • FIG. 1 is a schematic diagram of an apparatus and system for measuring lipid oxidation in lipid containing materials according to one embodiment of the presented technology.
  • FIG. 2 is a functional block diagram of a method for rapid lipid oxidation measurements and spoilage assessment of a sample according to one embodiment of the technology.
  • FIG. 3 is a plot comparing the sensor results of the TVOC sensor method and the conventional hexanal measurement using a gas chromatograph of the same sample.
  • FIG. 1 to FIG. 3 Several embodiments of the technology are described generally in FIG. 1 to FIG. 3 to illustrate the characteristics and functionality of the devices, systems, and methods. It will be appreciated that the methods may vary as to the specific steps and sequence and the systems and apparatus may vary as to structural details without departing from the basic concepts as disclosed herein. The method steps are merely exemplary of the order that these steps may occur. The steps may occur in any order that is desired, such that it still performs the goals of the claimed technology. Although a specific device architecture is used to illustrate the system, other structures and adaptations can be used to achieve the measurements and perform the sensing and calculating methods.
  • FIG. 1 the general structure of one apparatus and system 10 for measuring and assessing the content and the rate of change of volatile organic compounds is shown schematically. Because many food products emit more volatiles when they undergo spoilage, a measure of this increase in volatile production can indicate the present state of spoilage in food products.
  • the system and applied methods for measuring total volatile organic compounds (TVOC) provide an assessment of food spoilage based on measurements of volatiles (e.g. lipid oxidation) and rates of change of concentration as an indicator or proxy for food spoilage.
  • volatiles e.g. lipid oxidation
  • the apparatus 10 shown in FIG. 1 is particularly suited for measuring lipid oxidation in nuts, oils, and other lipid containing materials.
  • the apparatus 10 is generally built to measure the rate of volatile off gas accumulations as well as the rate of change of volatiles.
  • other lipid oxidation measurement methods and devices measure the equilibrium headspace for specific volatiles.
  • the apparatus 10 preferably measures the accumulation rate of volatiles, which enables faster assessments and nondestructive measurements.
  • the embodiment of the apparatus 10 shown schematically in FIG. 1 has four primary component parts including a sealed container 12 with lid 14, a sensor module 16, an air homogenizer 18, and a processing module 20 with a computer processor with programming for data receiving, processing and display.
  • Each sample is sealed in a container 12 with a lid 14 and volatiles from the sample begin to accumulate in the headspace over time.
  • Container size can be selected depending on sample size as well as sample type. A smaller headspace, for example, is advantageous in that it enables a faster accumulation of volatiles, leading to faster measurements and improved reproducibility.
  • the container 12 is preferably sized to accommodate the material being sampled and may be optimized for sensor 16 accuracy and efficiency.
  • the sensor module 16 of the apparatus 10 preferably has one or more TVOC sensors that may be the same type of sensor or a combination of different sensor types.
  • the sensor data received from sensors of distinct types can be compared or evaluated in parallel.
  • Suitable sensors 16 include sensors such as metal oxide semiconductors, photoionization detectors, and flame ionization detectors.
  • the sensors are connected to a transmitter that transmits sensor data to a remote receiver and computing device.
  • the sensor module 16 preferably measures total volatile organic compounds and preferably continuously measures the gas/volatiles and the rate of TVOC accumulation in the headspace of container 12 between the lid and the sample.
  • the processor module 20 receives data from the sensor module 14 and processes and displays and stores the results. Sensor data from the sensor module 16 is read and calculations are executed by a data processing of the processor module 20, which then outputs data, possibly to an LCD screen, computer, or transmits it to a mobile telephone with a transmitter, for example.
  • the processor module 20 of the apparatus includes one or more processors configured to receive input from the sensors and a non-transitory memory storing executable instructions for processing the received sensor data and other operations performed by the apparatus.
  • the processing module also includes a power source, user interface, an optional display and data storage.
  • This apparatus 10 is uniquely suited to executing rapid measurements based on the accumulation of volatiles in the headspace of a sealed container 12 over time.
  • Lipid oxidation measuring devices and methods known in the art generally aim to measure the concentration or amount of lipid oxidation products in a sample and are destructive processes. The measurement of the rate of volatile accumulation rather than just the concentration in the sample, permits an assessment of spoilage that is rapid and non-destructive in nature compared to conventional measurements.
  • the apparatus 10 preferably measures the total volatile organic compounds and accumulation rate, rather than distinguishing between specific volatiles using chromatography or by some other method.
  • the measurements of the total volatile organic compounds may then be used to determine a degree of spoilage or oxidation of the sample.
  • the measurements can also be used to provide a binary value such as “spoiled or not spoiled,” if the measured number or rate of accumulation exceeds a threshold, in another embodiment.
  • These numbers are also normally sample specific in that the degree of oxidation of one product may not indicate spoilage where the same degree would indicate spoilage in a different product.
  • An evaluation of the rate of change of volatiles may also indicate the remaining shelf life of the sample as well.
  • the TVOC system and method provided here uses no consumables, is nondestructive, and takes 3-5 minutes per sample.
  • the equipment cost is approximately $120 for a portable system with data logging capacity, user interface, and battery.
  • One caution for the TVOC system is that readings may be elevated by non-oxidation related volatiles such as aromas produced by some products, and cleaning detergent residues. Baseline readings and blanks can mitigate the effects of these confounding volatiles.
  • FIG. 2 One protocol 100 for TVOC measurements and spoilage state assessments according to the disclosed methods is shown in FIG. 2.
  • the container is optionally left open to the atmosphere for a period of time to allow the sensor readings to stabilize at block 110 in this illustration.
  • the sample for testing is placed in the analysis chamber or container and the lid or door is closed to seal the container or chamber.
  • the sample is left for a period of time to allow the volatile organic compounds from the sample to diffuse from the sample into the headspace between the sample and the lid or the free space in a chamber.
  • the VOC readings from the sensors are preferably monitored at block 130 and the rate of change will slow and stabilize. The amount of time may vary depending on the nature of the sample and the container dimensions.
  • Sensor readings are then taken at block 140 and the readings are analyzed by the processor.
  • the processed TVOC readings at block 140 are evaluated to assess the degree of spoilage as indicated by the rate of accumulation of TVOS’s. Such assessments are often specific to the type of sample that is evaluated.
  • the sensor signals may be acquired continuously or periodically at block 140 and recorded and stored for later processing or they may be processed contemporaneously. Processing of the signals at block 140 may also occur in a computer that is detached from the container from sensor signals or recordings transmitted from the container, in one embodiment.
  • the sensor data and assessment may be displayed and recorded completing the sample evaluation.
  • the container or chamber is then opened, and the sample is removed at block 150.
  • the TVOC measurement device shown generally in FIG. 1 was constructed and evaluated.
  • the system and method utilized a total volatile organic compounds (TVOC) sensor and a microcontroller or computer with GPIO pins, basic calculation capacity, and an ability to view or save data.
  • the system used for testing was the CCS811 MOX sensor and a raspberry pi system.
  • the CCS811 sensor is inserted into a sealed container with the sample to be analyzed and a small fan.
  • the computer calculated the rate of increase of TVOC concentration divided by the weight of the sample.
  • this measurement is well correlated with lipid oxidation in walnuts.
  • An ethanol solution in the range of 0.1 %-1 % can be used for standardization between analysis days. However, initial testing indicates that standardization between days is not necessary.
  • the system accurately predicted the order of the samples with regard to degree of oxidation.
  • this method can also be applied to ambient storage of nuts in an industrial setting.
  • Multiple CCS811 sensors can be connected to one controlling computer and placed inside multiple storage containers.
  • One sensor outside the containers can be used to account for normal changes in ambient volatiles.
  • the CCS811 sensor can be purchased for under $20 and is commonly available. This demonstrated the possibility of integrating many sensors in separate locations into one sensing system.
  • FIG. 3 shows a comparison of the proposed sensor TVOC method and hexanal measurement using a gas chromatograph.
  • Hexanal is a volatile product of lipid oxidation and is often used for lipid oxidation measurements.
  • the results shown in FIG. 3 and presented here demonstrated good agreement of the two methods with an overall Pearson’s correlation of 0.958.
  • the TVOC method was tested in oils and walnuts, and was well correlated with hexanal over a wide range of oxidation levels.
  • the device and methods will have many uses in the food industry for measuring oxidation and spoilage of raw materials, ingredients, and final products.
  • Raw materials measurable by this device include, but are not limited to, nuts, seeds, oils, and whole grains.
  • Ingredients measurable by this device include, but are not limited to, flours, oils, and fats.
  • Final products measurable by this device include, but are not limited to, fried foods, such as chips; baked products, such as crackers; and extruded foods, such as grain-based puffed snacks.
  • a lipid oxidation measurement apparatus comprising: (a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and (b) a computer processor connected to the one or more sensors configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
  • TVOC total volatile organic compound
  • the apparatus of any preceding or following implementation further comprising: a sealable container with an enclosed interior configured to hold a sample; and an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container; wherein the sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
  • a sealable container with an enclosed interior configured to hold a sample
  • an atmosphere homogenizer within the enclosed interior of the sealable container the homogenizer capable of agitating atmosphere within the interior of the container
  • the sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
  • TVOC total volatile organic compound
  • At least one sensor comprises one or more sensors selected from the group consisting of metal oxide semiconductors, photoionization detectors, and flame ionization detectors.
  • the computer processor further comprises a data storage device and a display.
  • the computer processor further comprises a transmitter capable of transmitting sensor accumulation and rate data to a remote receiver for storage.
  • An apparatus for measuring lipid oxidation in a sample comprising: (a) a sealable container with an enclosed interior configured to hold a sample; (b) at least one sensor configured to measure total volatile organic compounds (TVOC) or one or more component volatile organic compounds in the enclosed interior of the container; (c) one or more processors configured to receive input from the sensors; and (d) a non-transitory memory storing executable instructions that, if executed by the one or more processors, configure the apparatus to: (i) sense a quantity of volatile organic compounds within the enclosed interior of the container with one or more sensors; (ii) measure a rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors; (iii) record the sensor data in memory; and (e) assessing lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds.
  • TVOC total volatile organic compounds
  • sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
  • a method for measuring lipid oxidation in a sample comprising: (a) providing an open sealable container with an interior space capable of receiving a sample; (b) placing a sample within the container and sealing the container; (c) measuring a quantity of one or more volatile organic compounds within an enclosed interior of the container with at least one sensor; and (d) assessing lipid oxidation of a sample from the measured quantity of volatile organic compounds.
  • a food spoilage assessment apparatus comprising: (a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and (b) a transmitter capable of transmitting sensor data to a remote location for computer processing.
  • TVOC total volatile organic compound
  • the enclosed space comprises: a sealable container with an enclosed interior configured to hold a sample; wherein the sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
  • TVOC total volatile organic compound
  • sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
  • the apparatus of any preceding or following implementation further comprising: a computer processor operably connected to the at least one sensor configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
  • a computer processor operably connected to the at least one sensor configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
  • TVOC total volatile organic compounds
  • the computer processor further comprises: a data storage device; and a display.
  • a computer-implemented method for lipid oxidation measurement of a sample comprising: (a) acquiring a quantity of volatile organic compounds emitted from a sample; (b) measuring a concentration of volatile organic compounds; and (c) calculating lipid oxidation of the sample from the measured volatile organic compounds; (d) wherein said method is performed by one or more processors executing instructions stored on a non-transitory medium.
  • phrases “a,” “an,” and “the” may include plural referents unless the context clearly dictates otherwise. Reference to an object in the singular is not intended to mean “one and only one” unless explicitly so stated, but rather “one or more.”
  • Phrasing constructs, such as “A, B and/or C,” within the present disclosure describe where either A, B, or C can be present, or any combination of items A, B and C.
  • references in this disclosure referring to “an embodiment,” “at least one embodiment” or similar embodiment wording indicates that a particular feature, structure, or characteristic described in connection with a described embodiment is included in at least one embodiment of the present disclosure. Thus, these various embodiment phrases are not necessarily all referring to the same embodiment, or to a specific embodiment which differs from all the other embodiments being described.
  • the embodiment phrasing should be construed to mean that the particular features, structures, or characteristics of a given embodiment may be combined in any suitable manner in one or more embodiments of the disclosed apparatus, system or method.
  • a set refers to a collection of one or more objects.
  • a set of objects can include a single object or multiple objects.
  • Relational terms such as first and second, top and bottom, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.
  • a does not, without more constraints, preclude the existence of additional identical elements in the process, method, article, or apparatus that comprises, has, includes, contains the element.
  • the terms “approximately”, “approximate”, “substantially”, “essentially”, and “about”, or any other version thereof, are used to describe and account for small variations. When used in conjunction with an event or circumstance, the terms can refer to instances in which the event or circumstance occurs precisely as well as instances in which the event or circumstance occurs to a close approximation.
  • the terms can refer to a range of variation of less than or equal to ⁇ 10% of that numerical value, such as less than or equal to ⁇ 5%, less than or equal to ⁇ 4%, less than or equal to ⁇ 3%, less than or equal to ⁇ 2%, less than or equal to ⁇ 1 %, less than or equal to ⁇ 0.5%, less than or equal to ⁇ 0.1 %, or less than or equal to ⁇ 0.05%.
  • substantially aligned can refer to a range of angular variation of less than or equal to ⁇ 10°, such as less than or equal to ⁇ 5°, less than or equal to ⁇ 4°, less than or equal to ⁇ 3°, less than or equal to ⁇ 2°, less than or equal to ⁇ 1 °, less than or equal to ⁇ 0.5°, less than or equal to ⁇ 0.1 °, or less than or equal to ⁇ 0.05°.
  • range format is used for convenience and brevity and should be understood flexibly to include numerical values explicitly specified as limits of a range, but also to include all individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly specified.
  • a ratio in the range of about 1 to about 200 should be understood to include the explicitly recited limits of about 1 and about 200, but also to include individual ratios such as about 2, about 3, and about 4, and sub-ranges such as about 10 to about 50, about 20 to about 100, and so forth.
  • Coupled as used herein is defined as connected, although not necessarily directly and not necessarily mechanically.
  • a device or structure that is “configured” in a certain way is configured in at least that way but may also be configured in ways that are not listed.

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Abstract

Portable, inexpensive food spoilage assessment system and methods are provided that monitors and determines a state of spoilage or rancidity of stored foods with reduced time, labor and chemical inputs over conventional systems. The system and methods measure the rate of production or accumulation of organic volatiles (TVOC) from stored lipid products to measure lipid oxidation and are particularly suited for determining the oxidation of stored nuts, seeds, oils, and other lipid rich products. The apparatus has a sealed container, sensors, computer processor and mixing fan to take periodic or continuous measurements and rate determinations. The TVOC system and methods use no consumables, is nondestructive, and takes less than 5 minutes per sample with no sample preparation. The portable system enables lipid oxidation measurements in the storage facility and no outside lab, chemicals, or specialized knowledge are required.

Description

RAPID, LOW COST, VOLATILE ACCUMULATION SENSING INSTRUMENT FOR RANCIDITY MEASUREMENT IN NUTS AND OILS
CROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims priority to, and the benefit of, U.S. provisional patent application serial number 63/334,341 filed on April 25, 2022, incorporated herein by reference in its entirety. This application claims priority to, and the benefit of, U.S. provisional patent application serial number 63/334,507 filed on April 25, 2022, incorporated herein by reference in its entirety.
STATEMENT REGARDING FEDERALLY SPONSORED RESEARCH OR DEVELOPMENT
[0002] Not Applicable
NOTICE OF MATERIAL SUBJECT TO COPYRIGHT PROTECTION
[0003] A portion of the material in this patent document is subject to copyright protection under the copyright laws of the United States and of other countries. The owner of the copyright rights has no objection to the facsimile reproduction by anyone of the patent document or the patent disclosure, as it appears in the United States Patent and Trademark Office publicly available file or records, but otherwise reserves all copyright rights whatsoever. The copyright owner does not hereby waive any of its rights to have this patent document maintained in secrecy, including without limitation its rights pursuant to 37 C. F. R. § 1 .14.
BACKGROUND
[0004] 1. Technical Field
[0005] This technology pertains generally to systems and methods for the detection and quantification of spoilage or rancidity in foods and more particularly to inexpensive devices and methods for quickly measuring volatile organic compounds and the rate of change of accumulation as an assessment of spoilage.
[0006] 2. Background
[0007] Transportation and storage of perishable commodities may naturally lead to increasing degrees of spoilage over time. Producers benefit from spoilage assessments for ensuring profitability and food safety. For example, samples of perishable foods may be analyzed by techniques such as spectrophotometric assays, chromatographic assays, immunoassays and bacterial activity assays to determine spoilage.
[0008] The analysis of foods for contaminants or degradation products as an indicator of spoilage can be a complex task typically producing a time delay between the sampling and the receipt of results. During this delay, the content of indicators and the degree of spoilage may change leading to an erroneous assessment of spoilage or rancidity. In many instances, repeated sampling or continuous sampling and testing of a commodity is desirable to monitor daily changes or the rate of spoilage. Therefore, testing procedures that are accurate, quick and non-destructive are essential.
[0009] Many food products emit more volatiles when they undergo spoilage, such as milk, grains, fruits and vegetables. Measurements of this increase in volatile production can indicate a spoilage state in food products. For example, lipid oxidation is a significant contributor to food spoilage in high lipid content foods, such as nuts, seeds, and oils. Lipid oxidation is commonly measured throughout the food industry as a measure of spoilage. However, common oxidation measurements, including peroxide value, require high labor inputs, hazardous chemicals, and dedicated lab space. Current methods for lipid oxidation measurements include hexanal and peroxide value determination. While both are used regularly, each has drawbacks that can make obtaining results difficult, expensive, time consuming and unreliable.
[0010] For example, hexanal is a breakdown product of lipid oxidation that is typically measured using gas chromatography. Gas chromatography measurement of hexanal is reproducible and proportional to total lipid oxidation for most products but requires expensive (>$10,000) equipment and costly consumables as well as technically competent personnel. Additionally, the sample is often heated to release the volatiles, making gas chromatography a destructive method. A typical hexanal chromatography analysis of a sample typically requires about 45 minutes to run.
[0011] In comparison, a peroxide value is determined by well-established methods involving titration. Peroxide value measurements do not require specialized or expensive equipment. However, the process does involve significant chemical and labor inputs. A typical peroxide value determination by titration requires approximately 15 minutes per sample to run, produces hazardous chemical wastes, and is also a destructive method.
[0012] The largest disadvantage of the titration method for peroxide value determination is that it measures an intermediary product of oxidation rather than its chemical or labor requirements. As lipids oxidize, peroxide values increase as the amount of the intermediary compound increases, but then decreases as the intermediary compound further degrades. This process can cause erroneous data and conclusions in more extensively oxidized samples.
[0013] One example of a conventional system for peroxide measurement is the CDR FoodLab instrument, which costs between $4,000-$7,000, plus the cost of consumables. These rapid peroxide value methods still have the disadvantage of results that indicate decreasing peroxide values at a time when tested oils become highly oxidized.
[0014] Therefore a need exists for improved systems and methods for spoilage determination with reduced labor and chemical inputs over conventional systems that are low in cost, accurate and easy to operate.
BRIEF SUMMARY
[0015] A rapid, non-destructive, inexpensive system and method are provided that may be used for determining the oxidation of nuts, seeds, oils, and other lipid rich products as well as spoilage of other food products by microorganisms. This portable system can be used in warehouses, packing plants, and laboratories as an indicator of lipid oxidation and other types of spoilage. The system enables periodic or continuous monitoring of lipid oxidation during storage and rapid screening of perishable commodities upon receiving a shipment. [0016] The system and methods measure the rate of production or accumulation of organic volatiles (TVOC) from stored lipid containing products to measure lipid oxidation and other types of spoilage. This is an unconventional use of a total volatile organic compound sensor, which is typically used for air quality measurements. Additionally, the production rate of volatiles is measured instead of equilibrium headspace concentrations that are typically used for gas measurements. This allows for measurements in as little as 3 minutes per sample.
[0017] The TVOC system and methods of the technology use no consumables, is nondestructive, and takes about 1 minute to about 5 minutes per sample with no sample preparation requirements. The portable system enables lipid oxidation measurements in the storage facility and no lab, chemicals, or specialized knowledge are required. The equipment cost is approximately $120 for a portable system with data logging capacity, user interface, and battery. Preliminary results indicate accurate tracking of lipid oxidation trends in walnuts and olive oil. Validation is recommended for new product applications.
[0018] In one embodiment, an apparatus for measuring lipid oxidation in a sample is provided that has a sample container with sensors configured to measure total volatile organic compounds (TVOC) or one or more component volatile organic compounds in the enclosed interior of the container. The container preferably has a fan for agitating the atmosphere within the interior of the container to improve the accuracy of the sensors. The signals from the sensors are received and processed by a computer/ controller with software for sensing the quantity or concentration of volatile organic compounds and measuring rate of accumulation of total volatile organic compounds in the enclosed interior assessing lipid oxidation and the degree of spoilage of the sample. In one embodiment, the container includes a display for displaying the quantity and measured rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors as well as displaying the assessed lipid oxidation and degree of spoilage. In another embodiment, the computer is located remotely from the container and the sensor signals are transmitted from the container to the computer for processing. [0019] Several industries will benefit from the apparatus and methods. For example, the system would be useful for nut producers because nuts are highly susceptible to lipid oxidation and oxidation is one of the main drivers of reduced nut quality during storage. A ready to use analysis system based on this technology would allow for monitoring of nut lipid oxidation that is faster and less expensive than current methods. Similar to nuts, oxidation is a main driver of reduced oil quality during storage of many different food oils. A ready to use analysis system based on this technology would enable rapid, inexpensive testing of oil oxidation.
[0020] Companies that offer food analysis services and universities and research organizations may also benefit from this time and expense saving technology for oil and nut analysis.
[0021] Further aspects of the technology described herein will be brought out in the following portions of the specification, wherein the detailed description is for the purpose of fully disclosing preferred embodiments of the technology without placing limitations thereon.
BRIEF DESCRIPTION OF THE SEVERAL VIEWS OF THE DRAWINGS
[0022] The technology described herein will be more fully understood by reference to the following drawings which are for illustrative purposes only:
[0023] FIG. 1 is a schematic diagram of an apparatus and system for measuring lipid oxidation in lipid containing materials according to one embodiment of the presented technology.
[0024] FIG. 2 is a functional block diagram of a method for rapid lipid oxidation measurements and spoilage assessment of a sample according to one embodiment of the technology.
[0025] FIG. 3 is a plot comparing the sensor results of the TVOC sensor method and the conventional hexanal measurement using a gas chromatograph of the same sample.
DETAILED DESCRIPTION
[0026] Referring more specifically to the drawings, for illustrative purposes, systems and methods for quantifying spoilage or rancidity through periodic or continuous VOC measurements are generally shown. Several embodiments of the technology are described generally in FIG. 1 to FIG. 3 to illustrate the characteristics and functionality of the devices, systems, and methods. It will be appreciated that the methods may vary as to the specific steps and sequence and the systems and apparatus may vary as to structural details without departing from the basic concepts as disclosed herein. The method steps are merely exemplary of the order that these steps may occur. The steps may occur in any order that is desired, such that it still performs the goals of the claimed technology. Although a specific device architecture is used to illustrate the system, other structures and adaptations can be used to achieve the measurements and perform the sensing and calculating methods.
[0027] Turning now to FIG. 1 , the general structure of one apparatus and system 10 for measuring and assessing the content and the rate of change of volatile organic compounds is shown schematically. Because many food products emit more volatiles when they undergo spoilage, a measure of this increase in volatile production can indicate the present state of spoilage in food products. The system and applied methods for measuring total volatile organic compounds (TVOC) provide an assessment of food spoilage based on measurements of volatiles (e.g. lipid oxidation) and rates of change of concentration as an indicator or proxy for food spoilage.
[0028] The apparatus 10 shown in FIG. 1 is particularly suited for measuring lipid oxidation in nuts, oils, and other lipid containing materials. The apparatus 10 is generally built to measure the rate of volatile off gas accumulations as well as the rate of change of volatiles. In contrast, other lipid oxidation measurement methods and devices measure the equilibrium headspace for specific volatiles. The apparatus 10 preferably measures the accumulation rate of volatiles, which enables faster assessments and nondestructive measurements.
[0029] The embodiment of the apparatus 10 shown schematically in FIG. 1 has four primary component parts including a sealed container 12 with lid 14, a sensor module 16, an air homogenizer 18, and a processing module 20 with a computer processor with programming for data receiving, processing and display.
[0030] Each sample is sealed in a container 12 with a lid 14 and volatiles from the sample begin to accumulate in the headspace over time. Container size can be selected depending on sample size as well as sample type. A smaller headspace, for example, is advantageous in that it enables a faster accumulation of volatiles, leading to faster measurements and improved reproducibility. The container 12 is preferably sized to accommodate the material being sampled and may be optimized for sensor 16 accuracy and efficiency.
[0031] The sensor module 16 of the apparatus 10 preferably has one or more TVOC sensors that may be the same type of sensor or a combination of different sensor types. The sensor data received from sensors of distinct types can be compared or evaluated in parallel.
[0032] Suitable sensors 16 include sensors such as metal oxide semiconductors, photoionization detectors, and flame ionization detectors. In one embodiment, the sensors are connected to a transmitter that transmits sensor data to a remote receiver and computing device.
[0033] The sensor module 16 preferably measures total volatile organic compounds and preferably continuously measures the gas/volatiles and the rate of TVOC accumulation in the headspace of container 12 between the lid and the sample.
[0034] An air homogenizer 18, such as a fan, is preferably and optionally used to ensure that the volatiles produced by the sample are well mixed within the headspace of the sealed container 12 in this illustration. The mixing of the air and volatiles within the container improves the accuracy of the sensor measurements.
[0035] The processor module 20 receives data from the sensor module 14 and processes and displays and stores the results. Sensor data from the sensor module 16 is read and calculations are executed by a data processing of the processor module 20, which then outputs data, possibly to an LCD screen, computer, or transmits it to a mobile telephone with a transmitter, for example.
[0036] The processor module 20 of the apparatus includes one or more processors configured to receive input from the sensors and a non-transitory memory storing executable instructions for processing the received sensor data and other operations performed by the apparatus. The processing module also includes a power source, user interface, an optional display and data storage.
[0037] This apparatus 10 is uniquely suited to executing rapid measurements based on the accumulation of volatiles in the headspace of a sealed container 12 over time. Lipid oxidation measuring devices and methods known in the art generally aim to measure the concentration or amount of lipid oxidation products in a sample and are destructive processes. The measurement of the rate of volatile accumulation rather than just the concentration in the sample, permits an assessment of spoilage that is rapid and non-destructive in nature compared to conventional measurements.
[0038] In use, most samples can be placed in the interior of the container 12 with no preparation, which reduces total analysis time and allows for nondestructive measurements. Additionally, the apparatus 10 preferably measures the total volatile organic compounds and accumulation rate, rather than distinguishing between specific volatiles using chromatography or by some other method.
[0039] The measurements of the total volatile organic compounds may then be used to determine a degree of spoilage or oxidation of the sample. The measurements can also be used to provide a binary value such as “spoiled or not spoiled,” if the measured number or rate of accumulation exceeds a threshold, in another embodiment. These numbers are also normally sample specific in that the degree of oxidation of one product may not indicate spoilage where the same degree would indicate spoilage in a different product. An evaluation of the rate of change of volatiles may also indicate the remaining shelf life of the sample as well.
[0040] Accordingly, the TVOC system and method provided here uses no consumables, is nondestructive, and takes 3-5 minutes per sample. The equipment cost is approximately $120 for a portable system with data logging capacity, user interface, and battery. One caution for the TVOC system is that readings may be elevated by non-oxidation related volatiles such as aromas produced by some products, and cleaning detergent residues. Baseline readings and blanks can mitigate the effects of these confounding volatiles.
[0041] One protocol 100 for TVOC measurements and spoilage state assessments according to the disclosed methods is shown in FIG. 2. The container is optionally left open to the atmosphere for a period of time to allow the sensor readings to stabilize at block 110 in this illustration.
[0042] At block 120 the sample for testing is placed in the analysis chamber or container and the lid or door is closed to seal the container or chamber. The sample is left for a period of time to allow the volatile organic compounds from the sample to diffuse from the sample into the headspace between the sample and the lid or the free space in a chamber. The VOC readings from the sensors are preferably monitored at block 130 and the rate of change will slow and stabilize. The amount of time may vary depending on the nature of the sample and the container dimensions.
[0043] Sensor readings are then taken at block 140 and the readings are analyzed by the processor. The processed TVOC readings at block 140 are evaluated to assess the degree of spoilage as indicated by the rate of accumulation of TVOS’s. Such assessments are often specific to the type of sample that is evaluated. The sensor signals may be acquired continuously or periodically at block 140 and recorded and stored for later processing or they may be processed contemporaneously. Processing of the signals at block 140 may also occur in a computer that is detached from the container from sensor signals or recordings transmitted from the container, in one embodiment.
[0044] At block 150 the sensor data and assessment may be displayed and recorded completing the sample evaluation. The container or chamber is then opened, and the sample is removed at block 150.
[0045] The technology described herein may be better understood with reference to the accompanying examples, which are intended for purposes of illustration only and should not be construed as in any sense limiting the scope of the technology described herein as defined in the claims appended hereto. [0046] Example 1
[0047] In order to demonstrate the operational principles of the technology, a system was designed and validated. The TVOC measurement device shown generally in FIG. 1 was constructed and evaluated. The system and method utilized a total volatile organic compounds (TVOC) sensor and a microcontroller or computer with GPIO pins, basic calculation capacity, and an ability to view or save data. The system used for testing was the CCS811 MOX sensor and a raspberry pi system. The CCS811 sensor is inserted into a sealed container with the sample to be analyzed and a small fan. As the CCS811 measures the TVOC concentrations, the computer calculated the rate of increase of TVOC concentration divided by the weight of the sample. In preliminary testing, this measurement is well correlated with lipid oxidation in walnuts. An ethanol solution in the range of 0.1 %-1 % can be used for standardization between analysis days. However, initial testing indicates that standardization between days is not necessary. The system accurately predicted the order of the samples with regard to degree of oxidation.
[0048] In addition to the sealed container and method illustrated above, this method can also be applied to ambient storage of nuts in an industrial setting. For example, Multiple CCS811 sensors can be connected to one controlling computer and placed inside multiple storage containers. One sensor outside the containers can be used to account for normal changes in ambient volatiles. The CCS811 sensor can be purchased for under $20 and is commonly available. This demonstrated the possibility of integrating many sensors in separate locations into one sensing system.
[0049] Example 2
[0050] To further demonstrate the technology, the system and methods were tested and compared with the conventional hexanal measurements and spoilage estimations. FIG. 3 shows a comparison of the proposed sensor TVOC method and hexanal measurement using a gas chromatograph. Hexanal is a volatile product of lipid oxidation and is often used for lipid oxidation measurements. The results shown in FIG. 3 and presented here demonstrated good agreement of the two methods with an overall Pearson’s correlation of 0.958. [0051] As shown in FIG. 3, the TVOC method was tested in oils and walnuts, and was well correlated with hexanal over a wide range of oxidation levels.
[0052] The device and methods will have many uses in the food industry for measuring oxidation and spoilage of raw materials, ingredients, and final products. Raw materials measurable by this device include, but are not limited to, nuts, seeds, oils, and whole grains. Ingredients measurable by this device include, but are not limited to, flours, oils, and fats. Final products measurable by this device include, but are not limited to, fried foods, such as chips; baked products, such as crackers; and extruded foods, such as grain-based puffed snacks.
[0053] From the description herein, it will be appreciated that the present disclosure encompasses multiple embodiments which include, but are not limited to, the following:
[0054] A lipid oxidation measurement apparatus, comprising: (a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and (b) a computer processor connected to the one or more sensors configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
[0055] The apparatus of any preceding or following implementation, further comprising: a sealable container with an enclosed interior configured to hold a sample; and an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container; wherein the sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
[0056] The apparatus of any preceding or following implementation, wherein at least one sensor comprises one or more sensors selected from the group consisting of metal oxide semiconductors, photoionization detectors, and flame ionization detectors.
[0057] The apparatus of any preceding or following implementation, wherein the atmosphere homogenizer comprises a fan.
[0058] The apparatus of any preceding or following implementation, wherein the computer processor further comprises a data storage device and a display.
[0059] The apparatus of any preceding or following implementation, wherein the computer processor further comprises a transmitter capable of transmitting sensor accumulation and rate data to a remote receiver for storage.
[0060] An apparatus for measuring lipid oxidation in a sample, comprising: (a) a sealable container with an enclosed interior configured to hold a sample; (b) at least one sensor configured to measure total volatile organic compounds (TVOC) or one or more component volatile organic compounds in the enclosed interior of the container; (c) one or more processors configured to receive input from the sensors; and (d) a non-transitory memory storing executable instructions that, if executed by the one or more processors, configure the apparatus to: (i) sense a quantity of volatile organic compounds within the enclosed interior of the container with one or more sensors; (ii) measure a rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors; (iii) record the sensor data in memory; and (e) assessing lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds.
[0061] The apparatus of any preceding or following implementation, wherein the sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
[0062] The apparatus of any preceding or following implementation, wherein the instructions when executed by the processor further perform steps comprising: displaying the quantity and measured rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds on a display.
[0063] A method for measuring lipid oxidation in a sample, the method comprising: (a) providing an open sealable container with an interior space capable of receiving a sample; (b) placing a sample within the container and sealing the container; (c) measuring a quantity of one or more volatile organic compounds within an enclosed interior of the container with at least one sensor; and (d) assessing lipid oxidation of a sample from the measured quantity of volatile organic compounds.
[0064] The method of any preceding or following implementation, further comprising: measuring a rate of accumulation of one or more volatile organic compounds within the enclosed interior of the container; and assessing lipid oxidation of a sample from the measured rate of accumulation of volatile organic compounds.
[0065] The method of any preceding or following implementation, further comprising: waiting a period of time for sensors in the interior space of the sealed container to detect volatile organic compounds before measuring a quantity of volatile organic compounds.
[0066] The method of any preceding or following implementation, further comprising: providing a container with an air homogenizer; and agitating interior atmosphere within the enclosed interior of the container with the air homogenizer to mix any volatiles produced by a sample within the interior during sensor measurements.
[0067] The method of any preceding or following implementation, further comprising: providing a container with one or more TVOC sensors; and providing a transmitter coupled to the sensors, the transmitter capable of transmitting sensor data to a remote location for computer processing.
[0068] The method of any preceding or following implementation, further comprising: displaying the measured quantity and rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors on a display; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds on a display.
[0069] A food spoilage assessment apparatus, comprising: (a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and (b) a transmitter capable of transmitting sensor data to a remote location for computer processing.
[0070] The apparatus of any preceding or following implementation, wherein the enclosed space comprises: a sealable container with an enclosed interior configured to hold a sample; wherein the sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
[0071] The apparatus of any preceding or following implementation, wherein the sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
[0072] The apparatus of any preceding or following implementation, further comprising: a computer processor operably connected to the at least one sensor configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
[0073] The apparatus of any preceding or following implementation, wherein the computer processor further comprises: a data storage device; and a display.
[0074] A computer-implemented method for lipid oxidation measurement of a sample, the method comprising: (a) acquiring a quantity of volatile organic compounds emitted from a sample; (b) measuring a concentration of volatile organic compounds; and (c) calculating lipid oxidation of the sample from the measured volatile organic compounds; (d) wherein said method is performed by one or more processors executing instructions stored on a non-transitory medium.
[0075] The method of any preceding or following implementation, further comprising: displaying the concentration of total volatile organic compounds in the enclosed interior from the sensors on a display; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured volatile organic compounds on a display.
[0076] As used herein, the term "implementation" is intended to include, without limitation, embodiments, examples, or other forms of practicing the technology described herein.
[0077] As used herein, the singular terms "a," "an," and "the" may include plural referents unless the context clearly dictates otherwise. Reference to an object in the singular is not intended to mean "one and only one" unless explicitly so stated, but rather "one or more." [0078] Phrasing constructs, such as “A, B and/or C,” within the present disclosure describe where either A, B, or C can be present, or any combination of items A, B and C. Phrasing constructs indicating, such as “at least one of” followed by listing a group of elements, indicates that at least one of these group elements is present, which includes any possible combination of the listed elements as applicable.
[0079] References in this disclosure referring to “an embodiment,” “at least one embodiment” or similar embodiment wording indicates that a particular feature, structure, or characteristic described in connection with a described embodiment is included in at least one embodiment of the present disclosure. Thus, these various embodiment phrases are not necessarily all referring to the same embodiment, or to a specific embodiment which differs from all the other embodiments being described. The embodiment phrasing should be construed to mean that the particular features, structures, or characteristics of a given embodiment may be combined in any suitable manner in one or more embodiments of the disclosed apparatus, system or method.
[0080] As used herein, the term "set" refers to a collection of one or more objects. Thus, for example, a set of objects can include a single object or multiple objects.
[0081] Relational terms such as first and second, top and bottom, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions.
[0082] The terms "comprises," "comprising," "has", "having," "includes", "including," "contains", "containing" or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises, has, includes, contains a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. An element proceeded by "comprises . . . a", "has . . . a", "includes . . . a", "contains . . . a" does not, without more constraints, preclude the existence of additional identical elements in the process, method, article, or apparatus that comprises, has, includes, contains the element. [0083] As used herein, the terms "approximately", "approximate", "substantially", "essentially", and "about", or any other version thereof, are used to describe and account for small variations. When used in conjunction with an event or circumstance, the terms can refer to instances in which the event or circumstance occurs precisely as well as instances in which the event or circumstance occurs to a close approximation. When used in conjunction with a numerical value, the terms can refer to a range of variation of less than or equal to ± 10% of that numerical value, such as less than or equal to ±5%, less than or equal to ±4%, less than or equal to ±3%, less than or equal to ±2%, less than or equal to ±1 %, less than or equal to ±0.5%, less than or equal to ±0.1 %, or less than or equal to ±0.05%. For example, "substantially" aligned can refer to a range of angular variation of less than or equal to ±10°, such as less than or equal to ±5°, less than or equal to ±4°, less than or equal to ±3°, less than or equal to ±2°, less than or equal to ±1 °, less than or equal to ±0.5°, less than or equal to ±0.1 °, or less than or equal to ±0.05°.
[0084] Additionally, amounts, ratios, and other numerical values may sometimes be presented herein in a range format. It is to be understood that such range format is used for convenience and brevity and should be understood flexibly to include numerical values explicitly specified as limits of a range, but also to include all individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly specified. For example, a ratio in the range of about 1 to about 200 should be understood to include the explicitly recited limits of about 1 and about 200, but also to include individual ratios such as about 2, about 3, and about 4, and sub-ranges such as about 10 to about 50, about 20 to about 100, and so forth.
[0085] The term "coupled" as used herein is defined as connected, although not necessarily directly and not necessarily mechanically. A device or structure that is "configured" in a certain way is configured in at least that way but may also be configured in ways that are not listed.
[0086] Benefits, advantages, solutions to problems, and any element(s) that may cause any benefit, advantage, or solution to occur or become more pronounced are not to be construed as a critical, required, or essential features or elements of the technology describes herein or any or all the claims.
[0087] In addition, in the foregoing disclosure various features may grouped together in various embodiments for the purpose of streamlining the disclosure. This method of disclosure is not to be interpreted as reflecting an intention that the claimed embodiments require more features than are expressly recited in each claim. Inventive subject matter can lie in less than all features of a single disclosed embodiment.
[0088] The abstract of the disclosure is provided to allow the reader to quickly ascertain the nature of the technical disclosure. It is submitted with the understanding that it will not be used to interpret or limit the scope or meaning of the claims.
[0089] It will be appreciated that the practice of some jurisdictions may require deletion of one or more portions of the disclosure after that application is filed. Accordingly the reader should consult the application as filed for the original content of the disclosure. Any deletion of content of the disclosure should not be construed as a disclaimer, forfeiture or dedication to the public of any subject matter of the application as originally filed.
[0090] The following claims are hereby incorporated into the disclosure, with each claim standing on its own as a separately claimed subject matter.
[0091] Although the description herein contains many details, these should not be construed as limiting the scope of the disclosure but as merely providing illustrations of some of the presently preferred embodiments. Therefore, it will be appreciated that the scope of the disclosure fully encompasses other embodiments which may become obvious to those skilled in the art.
[0092] All structural and functional equivalents to the elements of the disclosed embodiments that are known to those of ordinary skill in the art are expressly incorporated herein by reference and are intended to be encompassed by the present claims. Furthermore, no element, component, or method step in the present disclosure is intended to be dedicated to the public regardless of whether the element, component, or method step is explicitly recited in the claims. No claim element herein is to be construed as a "means plus function" element unless the element is expressly recited using the phrase "means for". No claim element herein is to be construed as a "step plus function" element unless the element is expressly recited using the phrase "step for".

Claims

CLAIMS What is claimed is:
1 . A lipid oxidation measurement apparatus, comprising:
(a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and
(b) a computer processor connected to sensors configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
2. The apparatus of claim 1 , further comprising: a sealable container with an enclosed interior configured to hold a sample; and an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container; wherein said sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
3. The apparatus of claim 1 , wherein said at least one sensor comprises one or more sensors selected from the group consisting of metal oxide semiconductors, photoionization detectors, and flame ionization detectors.
4. The apparatus of claim 2, wherein the atmosphere homogenizer comprises a fan.
5. The apparatus of claim 1 , wherein said computer processor further comprises: a data storage device; and a display.
6. The apparatus of claim 1 , wherein said computer processor further comprises: a transmitter capable of transmitting sensor accumulation and rate data to a remote receiver for storage.
7. An apparatus for measuring lipid oxidation in a sample, comprising:
(a) a sealable container with an enclosed interior configured to hold a sample;
(b) at least one sensor configured to measure total volatile organic compounds (TVOC) or one or more component volatile organic compounds in the enclosed interior of the container;
(c) one or more processors configured to receive input from the sensors; and
(d) a non-transitory memory storing executable instructions that, if executed by the one or more processors, configure the apparatus to:
(i) sense a quantity of volatile organic compounds within the enclosed interior of the container with one or more sensors;
(ii) measure a rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors;
(iii) record the sensor data in memory; and
(e) assessing lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds.
8. The apparatus of claim 7, wherein said sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
9. The apparatus of claim 7, wherein said instructions when executed by the processor further perform steps comprising: displaying the quantity and measured rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds on a display.
10. A method for measuring lipid oxidation in a sample, the method comprising:
(a) providing an open sealable container with an interior space capable of receiving a sample;
(b) placing a sample within the container and sealing the container;
(c) measuring a quantity of one or more volatile organic compounds within an enclosed interior of the container with at least one sensor; and
(d) assessing lipid oxidation of a sample from the measured quantity of volatile organic compounds.
11 . The method of claim 10, further comprising: measuring a rate of accumulation of one or more volatile organic compounds within the enclosed interior of the container; and assessing lipid oxidation of a sample from the measured rate of accumulation of volatile organic compounds.
12. The method of claim 10, further comprising: waiting a period of time for sensors in the interior space of the sealed container to detect volatile organic compounds before measuring a quantity of volatile organic compounds.
13. The method of claim 10, further comprising: providing a container with an air homogenizer; and agitating interior atmosphere within the enclosed interior of the container with the air homogenizer to mix any volatiles produced by a sample within the interior during sensor measurements.
14. The method of claim 10, further comprising: providing a container with one or more TVOC sensors; and providing a transmitter coupled to said sensors, said transmitter capable of transmitting sensor data to a remote location for computer processing.
15. The method of claim 10, further comprising: displaying the measured quantity and rate of accumulation of total volatile organic compounds in the enclosed interior from the sensors on a display; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured rate of accumulation of volatile organic compounds on a display.
16. A food spoilage assessment apparatus, comprising:
(a) at least one sensor configured to measure total volatile organic compound (TVOC) in an enclosed space; and
(b) a transmitter capable of transmitting sensor data to a remote location for computer processing.
17. The apparatus of claim 16, wherein said enclosed space comprises: a sealable container with an enclosed interior configured to hold a sample; wherein said sensors are configured to measure total volatile organic compound (TVOC) in the enclosed interior of the sealable container.
18. The apparatus of claim 17, wherein said sealable container further comprises an atmosphere homogenizer within the enclosed interior of the sealable container, the homogenizer capable of agitating atmosphere within the interior of the container.
19. The apparatus of claim 16, further comprising: a computer processor operably connected to the at least one sensor configured to calculate a rate of accumulation of total volatile organic compounds (TVOC) as an indicator of lipid oxidation of a sample.
20. The apparatus of claim 19, wherein said computer processor further comprises: a data storage device; and a display.
21 . A computer-implemented method for lipid oxidation measurement of a sample, the method comprising:
(a) acquiring a quantity of volatile organic compounds emitted from a sample; (b) measuring a concentration of volatile organic compounds; and
(c) calculating lipid oxidation of the sample from the measured volatile organic compounds;
(d) wherein said method is performed by one or more processors executing instructions stored on a non-transitory medium.
22. The method of claim 21 , further comprising: displaying the concentration of total volatile organic compounds in the enclosed interior from the sensors on a display; and displaying assessed lipid oxidation and degree of spoilage of the sample from the measured volatile organic compounds on a display.
PCT/US2023/019670 2022-04-25 2023-04-24 Rapid, low cost, volatile accumulation sensing instrument for rancidity measurement in nuts and oils WO2023211862A1 (en)

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