WO2016176823A1 - 一种合成色素的检测方法及系统 - Google Patents

一种合成色素的检测方法及系统 Download PDF

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Publication number
WO2016176823A1
WO2016176823A1 PCT/CN2015/078273 CN2015078273W WO2016176823A1 WO 2016176823 A1 WO2016176823 A1 WO 2016176823A1 CN 2015078273 W CN2015078273 W CN 2015078273W WO 2016176823 A1 WO2016176823 A1 WO 2016176823A1
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pigment
information
searched
mass spectrometry
retrieved
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PCT/CN2015/078273
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English (en)
French (fr)
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马康
张庆合
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中国计量科学研究院
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Priority to PCT/CN2015/078273 priority Critical patent/WO2016176823A1/zh
Publication of WO2016176823A1 publication Critical patent/WO2016176823A1/zh

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/64—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber

Definitions

  • the present application relates to the field of analytical chemistry, and in particular to a method and system for detecting synthetic pigments.
  • Pigments are widely used in the food industry as a common additive. Adding pigments can improve the color quality of foods, thereby increasing the added value of foods. According to the source, pigments can be divided into natural pigments and synthetic pigments. Natural pigments have high safety, but the coloring effect is poor and the price is high, which is less used in the food industry. Synthetic pigments are widely used in the food industry because of their good tinting strength, fading, and low cost.
  • These synthetic dyes such as industrial dyes, are mostly made from aromatic hydrocarbons such as benzene, toluene, and naphthalene, and are synthesized by a series of organic reactions such as sulfonation, nitration, halogenation, azotization, etc., and most of them are azo compounds in the body. Internal biotransformation can form carcinogens. At the same time, impurities such as arsenic, mercury, phenol, aniline, lead, cadmium, ether, chloride, sulfate, etc. produced during the synthesis process have different degrees of toxicity, which will seriously affect the health of consumers. Therefore, the abuse of synthetic dyes such as industrial dyes is more harmful. In the food testing process after food safety problems, it is necessary to quickly and effectively detect the synthetic pigments contained in foods, so as to timely adopt corresponding treatment measures to reduce food safety. The hazard of the problem.
  • the detection method of the synthetic pigment contained in the food is usually analyzed by various complicated tests to analyze the components contained in the food sample, and the type of the synthetic pigment contained in the food cannot be quickly screened, resulting in a sudden
  • the detection speed of the synthetic pigment contained in the food is too slow. Therefore, the harm caused by food safety problems cannot be quickly and effectively reduced.
  • the embodiments of the present application provide a method and system for detecting synthetic pigments, which are used to quickly screen the types of synthetic pigments contained in foods, thereby timely adopting corresponding treatment measures to reduce the hazards of food safety problems.
  • a method for detecting a synthetic pigment for detecting a pigment to be retrieved in a food sample comprising:
  • the physicochemical property information includes: a pigment name, a CAS number, a molecular formula, a molecular weight, a molecular structure, and a color index.
  • the method for establishing the pigment database comprises:
  • the physical property information data, the spectral information database, and the multi-stage mass spectrometry information database are combined into the pigment database.
  • the acquiring the spectral information of the pigment to be retrieved comprises:
  • a wavelength range for scanning the dye to be searched to cover (200-700) nm of the visible light region and the ultraviolet light region, a scanning speed of 120 nm/min, and a slit width of 0.2 nm;
  • the acquiring the multi-stage mass spectrometry information of the pigment to be retrieved comprises:
  • the ion peak interval of the pigment to be searched is collected as a spectral information of the pigment to be searched in a scanning range of (10-1000) m/z.
  • the method further comprises:
  • the pigment information includes: a pigment name, a molecular structure, a spectral information map, a multi-stage mass spectrometry information map, a reference detection standard, and a reference detection method And references.
  • the application also provides a detection system for synthetic pigments for detecting pigments to be retrieved in a food sample, including:
  • a physicochemical property information detecting module configured to acquire at least one physicochemical property information of the pigment to be searched in the food sample, and determine the pigment to be retrieved in a pre-established pigment database according to the at least one physicochemical property information The waiting range to be retrieved;
  • a spectral information detecting module configured to acquire spectral information of the pigment to be retrieved, and perform rough search in the to-be-searched interval according to the spectral information to obtain at least one rough search result
  • a mass spectrometry information detecting module configured to acquire multi-stage mass spectrometry information of the pigment to be retrieved, and perform exact matching in the at least one rough search result according to the multi-stage mass spectrometry information to determine an exact match of the pigment to be retrieved result.
  • the physicochemical property information includes: a pigment name, a CAS number, a molecular formula, a molecular weight, a molecular structure, and a color index.
  • the pre-established pigment database comprises:
  • a physicochemical property information data module for analyzing physicochemical property information of a plurality of standard pigments, and establishing a physical property information database according to the mapping relationship between the physicochemical property information and the corresponding standard pigment;
  • a spectral information data module for performing spectral scanning on a plurality of standard pigments, collecting spectral information of a plurality of standard pigments, and establishing a spectral information database according to the mapping relationship between the spectral information and the corresponding standard pigment;
  • a mass spectrometry information data module for performing mass spectrometry on a plurality of standard pigments to obtain multi-stage mass spectrometry information of a plurality of standard pigments, and establishing a multi-stage mass spectrometry information database according to the mapping relationship between the multi-stage mass spectrometry information and the corresponding standard pigment;
  • a pigment data merging module for merging the physicochemical property information data, the spectral information database, and the multi-stage mass spectrometry information database into the pigment database.
  • the method further comprises:
  • a pigment information output module configured to output pigment information of the pigment to be searched according to an exact matching result of the pigment to be searched;
  • the pigment information includes: a pigment name, a molecular structure, a spectral information map, a multi-stage mass spectrometry information map, Reference test standards, reference test methods, and references.
  • the existing known standard pigments can be analyzed, the pigment database is pre-established according to the obtained physicochemical property information and the spectrum map, and then the rough search interval is determined by the physicochemical property information and the spectral information, and the pigment to be searched is narrowed in the pigment database.
  • the search range, and then through the multi-level mass spectrometry information to obtain accurate detection results the hierarchical progressive search method can not only reduce the workload of retrieval, but also quickly and accurately detect the types of pigments to be retrieved, reduce the screening error, and finally achieve Fast and accurate detection of pigment categories to improve response to sudden food safety incidents.
  • Example 1 is a flow chart of a method for detecting a synthetic dye provided in Example 1 of the present application;
  • Example 2 is a flow chart of a method for detecting a synthetic dye provided in Example 2 of the present application;
  • Example 3 is a flow chart of a method for detecting a synthetic dye provided in Example 3 of the present application.
  • Example 4 is a schematic structural view of a detection system for a synthetic pigment provided in Example 4 of the present application;
  • Example 5 is a schematic structural view of a detection system for a synthetic pigment provided in Example 5 of the present application.
  • Example 6 is a schematic structural view of a detection system for a synthetic pigment provided in Example 6 of the present application.
  • Embodiment 1 is a diagrammatic representation of Embodiment 1:
  • Example 1 is a flow chart of a method for detecting a synthetic dye provided in Example 1 of the present application.
  • a method for detecting a synthetic pigment provided in an embodiment of the present application is used for detecting a type of a pigment to be searched in a food sample.
  • the method for detecting a synthetic pigment provided by the embodiment of the present application includes:
  • Step S11 Obtain at least one physical property information of the color to be retrieved in the food sample, and determine a to-be-searched interval of the color to be retrieved in a pre-established pigment database according to the at least one physical property information.
  • the applicant can summarize the pigments appearing in the literature and the standard by studying the synthetic pigment articles published in recent domestic and foreign journals, and the synthetic pigment standards currently in use, and the pre-established pigment database. .
  • Use pigment name, detection method, substrate, detection limit Different system identification and differentiation.
  • the high-frequency pigments are preferentially built, and the key physicochemical properties such as name, CAS number, molecular formula and color index are also systematically identified and distinguished in the pigment database. It is also possible to determine among the possible physicochemical properties parameters a unique correspondence between a type of parameter and a synthetic pigment, and to identify the number in the database.
  • the two parameters of CAS number and color index are clear and easy to check compared with the molecular weight of the molecular formula. Therefore, these two parameters can be recorded as key parameters to improve the convenience of detection and application of the pigment database.
  • the color index as a physical parameter of the synthetic pigment, embodies the special property of the pigment to absorb a specific wavelength range in the visible light region, and the specific color is produced. In the development of instrument detection methods, this property is utilized. most.
  • the pigment database may also include general physicochemical properties such as common Chinese and English names, molecular formulas, molecular weights, molecular structures, melting points, uses, and main sources of pigments.
  • the physicochemical property information of the pigment to be retrieved can be collected by the instrument and then input into the pigment database, and the corresponding interval to be retrieved can be obtained from the database.
  • the search can be performed by Chinese and English names, CAS numbers, molecular formulas, molecular weights, color indexes, and the like. For example, if the carbon number of the pigment to be searched is 20, the corresponding searched interval may be obtained by searching in the pigment database: C20; or if the color index (CI) of the pigment to be searched is 45,430, the color index is searched. You can get the interval to be searched.
  • Step S12 Acquire the spectral information of the pigment to be retrieved, and perform a rough search in the to-be-searched interval according to the spectral information to obtain at least one rough search result.
  • the rough search result may be retrieved from the to-be-searched interval according to the spectral information of the pigment to be retrieved. For example, if the absorption peak of the dye to be searched in the visible light region is around 530 nm, the search result can be searched in the interval to be searched to obtain a rough search result, thereby achieving the purpose of narrowing the search interval, and the search accuracy is further improved.
  • the wavelength range is set to (200 to 700) nm, the scanning speed is 120 nm/min, and the slit width is 0.2 nm.
  • the pure pigment is weighed and then formulated into a solution with a solvent (water/methanol). It is preferably formulated into a solution using 100% methanol.
  • a solvent water/methanol
  • the partially synthesized pigment is insoluble in methanol, it is prepared by using 100% water as a solvent.
  • the concentration of the synthetic pigment is adjusted within the range of (5-40) ⁇ 10 -6 by appropriately adjusting the concentration of the solution, so that the characteristic absorption peak of the visible light region in the spectral data is absorbed.
  • the value is controlled near (0.6 to 1.0).
  • Step S13 Acquire multi-stage mass spectrometry information of the pigment to be retrieved, and perform exact matching in the at least one rough search result according to the multi-stage mass spectrometry information to determine an exact matching result of the pigment to be retrieved.
  • the physicochemical property information and the spectral information retrieval of the pigment to be retrieved can narrow the search range and reduce the workload of the retrieval.
  • the multi-level mass spectrometry information of the pigment to be retrieved can be used for retrieval.
  • the MS 1 information is not highly matched by the substrate environment and the pre-processing, and it is difficult to ensure the accuracy of the screening.
  • the introduction of MS 2 and MS 3 ensures the accuracy of the screening results, thereby utilizing the pigment to be retrieved. It is very necessary to search the multi-stage mass spectrometry information in the pigment database.
  • the multi-stage mass spectrometry information stored in the pigment database can improve the retrieval precision and reduce the qualitative error of the pigment to be searched.
  • the instrument uses the ESI source and is fully tuned before use, using the default instrument parameters, including: CDL temperature: 200 ° C; Heat Block temperature: 200 ° C; dry gas Flow rate: 1.5 L/min; detection voltage: 1.58 kV; Interface voltage (+): 4.5 kV; Interfce voltage (-): -3.5 kV; scanning range: (100-1000) m/z.
  • the buffered salt solution of methanol and water is used.
  • the proportion of methanol in the mobile phase is generally 80%-100%.
  • the present application preferably uses 0.1% formic acid-10 mmol of the amine acetate-water solution and 100%.
  • % methanol was used as the mobile phase of the mass spectrometer in a ratio of 10:90. Under this mobile phase, all kinds of synthetic pigments have a good response. After the pure product is weighed, it is preferentially diluted to 10 mg/L or less with 100% methanol, and the injection amount is 5 ⁇ l. The sample does not pass through the column and goes directly to the mass spectrometer for analysis. Multi-level mass spectrometry error The difference satisfies the requirements of the application and provides a basis for the precise determination of the type of pigment to be retrieved.
  • the difference in the structure and properties of the synthetic pigment determines whether the mass spectrometry data is acquired in positive ion mode or negative ion mode.
  • all the dyes to be tested are scanned in two modes, and the best ion response is selected.
  • the model performs further data collection.
  • the existing known standard pigments can be analyzed, the pigment database is pre-established according to the obtained physicochemical property information and the spectrum map, and then the rough search interval is determined by the physicochemical property information and the spectral information, and the pigment to be searched is narrowed in the pigment database.
  • the search range, and then through the multi-level mass spectrometry information to obtain accurate detection results the hierarchical progressive search method can not only reduce the workload of retrieval, but also quickly and accurately detect the types of pigments to be retrieved, reduce the screening error, and finally achieve Fast and accurate detection of pigment categories to improve response to sudden food safety incidents.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • Example 2 is a flow chart of a method for detecting a synthetic dye provided in Example 2 of the present application.
  • a method for detecting a synthetic pigment provided in an embodiment of the present invention is used for detecting a type of a pigment to be searched in a food sample.
  • the method for detecting a synthetic pigment provided in an embodiment of the present application includes The following steps:
  • Step S21 analyzing the physical property information of the plurality of standard pigments, and establishing a physical property information database according to the mapping relationship between the physical property information and the corresponding standard pigment.
  • Step S22 performing spectral scanning on a plurality of standard pigments, collecting spectral information of a plurality of standard pigments, and establishing a spectral information database according to the mapping relationship between the spectral information and the corresponding standard pigment.
  • Step S23 performing mass spectrometry on a plurality of standard pigments to obtain multi-stage mass spectrometry information of a plurality of standard pigments, and establishing a multi-stage mass spectrometry information database according to the mapping relationship between the multi-stage mass spectrometry information and the corresponding standard pigment.
  • Step S24 Combining the physical property information data, the spectral information database, and the multi-stage mass spectrometry information database into the pigment database.
  • the physicochemical property information, the spectral information, and the multi-stage mass spectrometry information of the obtained standard pigment are introduced into the database software of ACD/Labs, and the pigment database is established in units of pigments.
  • ACD/Labs combines the information of each part into a whole.
  • the information of each pigment forms a unit.
  • Each unit has the necessary information of pigment, such as Chinese and English name, CAS number, color index, molecular formula, molecular structure, spectral information, Multi-level mass spectrometry information, etc.
  • the standard pigment in the pigment database can be matched and the type of the pigment to be searched can be obtained.
  • the existing known standard pigments can be analyzed, the pigment database is pre-established according to the obtained physicochemical property information and the spectrum map, and then the rough search interval is determined by the physicochemical property information and the spectral information, and the pigment to be searched is narrowed in the pigment database.
  • the search range, and then through the multi-level mass spectrometry information to obtain accurate detection results the hierarchical progressive search method can not only reduce the workload of retrieval, but also quickly and accurately detect the types of pigments to be retrieved, reduce the screening error, and finally achieve Fast and accurate detection of pigment categories to improve response to sudden food safety incidents.
  • Embodiment 3 is a diagrammatic representation of Embodiment 3
  • Example 3 is a flow chart of a method for detecting a synthetic dye provided in Example 3 of the present application.
  • a method for detecting a synthetic pigment provided in an embodiment of the present application is for detecting a type of a pigment to be retrieved in a food sample, and includes the following steps:
  • Step S11 Obtaining at least one physicochemical property information of the pigment to be retrieved in the food sample, and determining the to-be-checked in a pre-established pigment database according to the at least one physicochemical property information The interval to be searched for.
  • Step S12 Acquire the spectral information of the pigment to be retrieved, and perform a rough search in the to-be-searched interval according to the spectral information to obtain at least one rough search result.
  • Step S13 Acquire multi-stage mass spectrometry information of the pigment to be retrieved, and perform exact matching in the at least one rough search result according to the multi-stage mass spectrometry information to determine an exact matching result of the pigment to be retrieved.
  • Step S14 outputting the pigment information of the pigment to be searched according to the exact matching result of the pigment to be retrieved;
  • the pigment information includes: a pigment name, a molecular structure, a spectral information map, a multi-stage mass spectrometry information map, a reference detection standard, Reference test methods and references.
  • the pigment database can provide detailed information about the pigment to the searcher: including physical information such as name and molecular structure, spectral map, multi-stage mass spectrum, literature and standards. Wait. At this time, it is convenient to carry out related research work after rapid screening. For example, after confirming erythrosin by mass spectrometry, its cleavage pathway can be determined by spectroscopic processing software and references, and domestic detection methods related to the pigment can also be found. These efforts facilitate the research of pigments and respond quickly to sudden food safety incidents.
  • the existing known standard pigments can be analyzed, the pigment database is pre-established based on the obtained physicochemical property information and spectral information, and the multi-stage mass spectrometry information, and then the rough search interval is determined by the physicochemical property information and the spectral information, and the pigment to be searched is narrowed.
  • the accurate detection results are obtained through multi-stage mass spectrometry information, and the hierarchical progressive search method can not only reduce the workload of the search, but also quickly and accurately detect the types of pigments to be retrieved and reduce the sieve. Check the error, and finally achieve fast and accurate detection of the pigment category, and improve the response speed to sudden food safety incidents.
  • the invention discloses a method for detecting a synthetic pigment, and correspondingly, the invention also discloses a system for applying the above-mentioned method for detecting a synthetic pigment, which is used for realizing rapid and accurate detection of a pigment type and improving a safety event for a sudden food. responding speed.
  • Embodiment 4 is a diagrammatic representation of Embodiment 4:
  • Example 4 is a schematic structural view of a detection system for a synthetic pigment provided in Example 4 of the present application.
  • a detection system for a synthetic pigment provided in an embodiment of the present application is for detecting a type of a pigment to be retrieved in a food sample, including:
  • the physicochemical property information detecting module 1 is configured to acquire at least one physicochemical property information of the pigment to be searched in the food sample, and determine the to-be-searched in a pre-established pigment database according to the at least one physicochemical property information The interval to be retrieved from the pigment.
  • ACD/Labs can be used to establish the pigment database, and the pigment database is commonly used for data support of liquid chromatography tandem mass spectrometry instruments of different types and different principles.
  • the source of the standard pigments involved in the pigment database may be Chem Service and the China National Standards Development Center. Information on the physicochemical properties of standard pigments can be obtained by authoritative chemical literature searches.
  • the spectral information detecting module 2 is configured to acquire spectral information of the pigment to be retrieved, and perform rough search in the to-be-searched interval according to the spectral information to obtain at least one rough search result.
  • the spectral information of the pigment to be retrieved can be acquired by the Hitachi U-3900 ultraviolet visible spectrometer.
  • a mass spectrometry information detecting module 3 configured to acquire multi-stage mass spectrometry information of the pigment to be retrieved, and perform exact matching in the at least one rough search result according to the multi-stage mass spectrometry information to determine an accuracy of the pigment to be retrieved Match the result.
  • the multi-stage mass spectrometry information of the pigment to be retrieved can be acquired by the Shimadzu LCMS-IT-TOF ion capture time-of-flight mass spectrometer. Compared with other mass spectrometers, it has the advantages of high precision, multi-stage mass spectrometry, high detection speed, etc. These features are highly consistent with the requirements of the pigment database application, so it is selected as a mass spectrometer for data acquisition.
  • the information transmission method in the foregoing method embodiment may be used in the electronic device provided by the embodiment of the present application, and details are not described herein again.
  • Embodiment 5 is a diagrammatic representation of Embodiment 5:
  • FIG. 5 is a schematic structural view of a detection system for a synthetic pigment provided in Example 5 of the present application.
  • a detection system for a synthetic pigment provided in an embodiment of the present application is for detecting a type of a pigment to be retrieved in a food sample, wherein the system for establishing a pigment database includes:
  • the physicochemical property information data module 11 is configured to analyze the physicochemical property information of the plurality of standard pigments, and establish a physical property information database according to the mapping relationship between the physicochemical property information and the corresponding standard pigment;
  • the spectral information data module 12 is configured to perform spectral scanning on a plurality of standard pigments, collect spectral information of a plurality of standard pigments, and establish a spectral information database according to the mapping relationship between the spectral information and the corresponding standard pigment;
  • the mass spectrometry information data module 13 is configured to perform mass spectrometry on a plurality of standard pigments to obtain multi-stage mass spectrometry information of a plurality of standard pigments, and establish a multi-stage mass spectrometry information database according to the mapping relationship between the multi-stage mass spectrometry information and the corresponding standard pigments. ;
  • the pigment data merging module 14 is configured to merge the physicochemical property information data, the spectral information database, and the multi-stage mass spectrometry information database into the pigment database.
  • the information transmission method in the foregoing method embodiment may be used in the electronic device provided by the embodiment of the present application, and details are not described herein again.
  • Example 6 is a schematic structural view of a detection system for a synthetic pigment provided in Example 6 of the present application.
  • a detection system for a synthetic pigment provided in an embodiment of the present application is used for detecting a type of a pigment to be retrieved in a food sample, including:
  • the physicochemical property information detecting module 1 is configured to acquire at least one physicochemical property information of the pigment to be searched in the food sample, and determine the to-be-searched in a pre-established pigment database according to the at least one physicochemical property information The interval to be retrieved from the pigment.
  • the establishment of the pigment database can use ACD/Labs, the pigment database.
  • the source of the standard pigments involved in the pigment database may be Chem Service and the China National Standards Development Center. Information on the physicochemical properties of standard pigments can be obtained by authoritative chemical literature searches.
  • the spectral information detecting module 2 is configured to acquire spectral information of the pigment to be retrieved, and perform rough search in the to-be-searched interval according to the spectral information to obtain at least one rough search result.
  • the spectral information of the pigment to be retrieved can be acquired by the Hitachi U-3900 ultraviolet visible spectrometer.
  • a mass spectrometry information detecting module 3 configured to acquire multi-stage mass spectrometry information of the pigment to be retrieved, and perform exact matching in the at least one rough search result according to the multi-stage mass spectrometry information to determine an accuracy of the pigment to be retrieved Match the result.
  • the multi-stage mass spectrometry information of the pigment to be retrieved can be acquired by the Shimadzu LCMS-IT-TOF ion capture time-of-flight mass spectrometer. Compared with other mass spectrometers, it has the advantages of high precision, multi-stage mass spectrometry, high detection speed, etc. These features are highly consistent with the requirements of the pigment database application, so it is selected as a mass spectrometer for data acquisition.
  • the pigment information output module 4 is configured to output the pigment information of the pigment to be searched according to the exact matching result of the pigment to be retrieved; the pigment information includes: a pigment name, a molecular structure, a spectral information map, and a multi-stage mass spectrometry information map. , reference test standards, reference test methods and references.
  • the information transmission method in the foregoing method embodiment may be used in the electronic device provided by the embodiment of the present application, and details are not described herein again.
  • the existing known standard pigments can be analyzed, the pigment database is pre-established based on the obtained physicochemical property information and spectral information, and the multi-stage mass spectrometry information, and then the rough search interval is determined by the physicochemical property information and the spectral information, and the pigment to be searched is narrowed.
  • Number of pigments According to the search range in the library, the accurate detection results are obtained through multi-level mass spectrometry information, and the hierarchical progressive search method can not only reduce the workload of the search, but also quickly and accurately detect the types of pigments to be searched and reduce the screening. The error finally achieves fast and accurate detection of the pigment category and improves the response speed to sudden food safety incidents.
  • the steps of a method or algorithm described in connection with the embodiments disclosed herein can be implemented directly in hardware, a software module executed by a processor, or a combination of both.
  • the software module can be placed in random access memory (RAM), memory, read only memory (ROM), electrically programmable ROM, electrically erasable programmable ROM, registers, hard disk, removable disk, CD-ROM, or technical field. Any other form of storage medium known.

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Abstract

一种合成色素的检测方法，获取食品样品中的待检索色素的至少一种物化性质信息，并根据至少一种物化性质信息，在预先建立的色素数据库中确定待检索色素的待检索区间；获取待检索色素的光谱信息，并根据光谱信息，在待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取待检索色素的多级质谱信息，并根据多级质谱信息，在至少一个粗略检索结果中进行精确匹配，确定待检索色素的精确匹配结果。预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，再通过多级质谱信息得到精确的检测结果，可以减少检索的工作量，快速准确地检测出待检索色素的种类，进而提高对突发食品安全事件的响应速度。

Description

一种合成色素的检测方法及系统 技术领域
本申请涉及分析化学技术领域，特别是涉及一种合成色素的检测方法及系统。
背景技术
随着生活水平的提高，人们越来越关系食品安全问题。色素作为一种常见添加剂在食品行业中应用广泛。添加色素可以改善食品的色泽品质，以此提高食品的附加值。色素按照来源可分为天然色素和合成色素两类，天然色素安全性高，但是着色效果差、价格较高，在食品行业中应用较少。合成色素的特点是着色力好、不易褪色、成本低，因此在食品行业中应用广泛。
合成色素的种类很多，但是合成色素的滥用会严重危害到人类尤其是儿童的身体健康，因此各国对食品中的合成色素的使用范围和使用量都有所规定，不在规定内的合成色素均不能作为食品添加剂出现在食品中。而近年来，食品安全问题风波不断，化学添加剂违规添加或超标添加等问题的频频发生，一些商家由于经济利益驱使，会在食品中添加一些工业染料等合成色素，例如苏丹红、碱性橙、碱性嫩黄等，造成了重大人身伤亡和财产损失，危害了人们的身心健康，使食品安全问题愈加成为全社会关注的热点。这些工业染料等合成色素多以苯、甲苯、萘等芳烃类化工产品为原料，经过磺化、硝化、卤化、偶氮化等一系列有机反应化合而成，且多数属偶氮化合物，在机体内经生物转化，可形成致癌物。同时在合成过程中产生的杂质如砷、汞、苯酚、苯胺、铅、镉、乙醚、氯化物、硫酸盐等均有不同程度的毒性，会严重影响消费者的健康。因此，滥用工业染料等合成色素造成的危害更大，在食品安全问题发生后的食品检测过程中，需要快速有效地检测食品中所含的合成色素，从而及时采用相应的治疗措施来减少食品安全问题的危害。
但是，目前对于食品中所含的合成色素的检测方法，通常是通过各类复杂试验来分析食品样品中所含的成分，不能快速筛查食品中所含的合成色素的种类，导致在突发食品安全问题时，对于食品中所含的合成色素的检测速度过慢， 从而不能快速有效地减少食品安全问题带来的危害。
发明内容
有鉴于此，本申请实施例提供一种合成色素的检测方法及系统，以对食品中所含的合成色素的种类进行快速筛查，从而及时采用相应的治疗措施来减少食品安全问题的危害。
为了实现上述目的，本申请实施例提供的技术方案如下：
一种合成色素的检测方法，用于检测食品样本中的待检索色素，包括：
获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；
获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；
获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
优选地，所述物化性质信息，包括：色素名称、CAS号、分子式、分子量、分子结构和色指数。
优选地，所述色素数据库的建立方法包括：
分析多种标准色素的物化性质信息，并根据所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库；
对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库；
对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库；
将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
优选地，所述获取所述待检索色素的光谱信息，包括：
以100％甲醇或100％水作为溶剂，配制所述待检索色素的溶液，使所述 待检索色素的溶液浓度在(5～40)×10-6范围内；
设置扫描所述待检索色素的波长范围为覆盖可见光区和紫外光区的(200～700)nm，扫描速度为120nm/min，狭缝宽度为0.2nm；
采集所述待检索色素的吸收波峰，并将所述吸收波峰作为所述待检索色素的光谱信息。
优选地，所述获取所述待检索色素的多级质谱信息，包括：
以100％甲醇或100％水作为溶剂，配制所述待检索色素的溶液；
以0.1％甲酸-10mmol乙酸胺-水溶液和100％甲醇作为流动相，且所述流动相中的甲醇的比例在80％-100％范围内；
以(10-1000)m/z的扫描范围采集所述待检索色素的离子峰区间，作为所述待检索色素的光谱信息。
优选地，还包括：
根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
本申请还提供一种合成色素的检测系统，用于检测食品样本中的待检索色素，包括：
物化性质信息检测模块，用于获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；
光谱信息检测模块，用于获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；
质谱信息检测模块，用于获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
优选地，所述物化性质信息，包括：色素名称、CAS号、分子式、分子量、分子结构和色指数。
优选地，所述预先建立的色素数据库，包括：
物化性质信息数据模块，用于分析多种标准色素的物化性质信息，并根据所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库；
光谱信息数据模块，用于对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库；
质谱信息数据模块，用于对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库；
色素数据合并模块，用于将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
优选地，还包括：
色素信息输出模块，用于根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
应用本申请提供的一种合成色素的检测方法及系统，获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。这样，可以对现存已知的标准色素进行分析，根据得到的物化性质信息和谱图预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，缩小待检索色素在色素数据库中的检索范围，再通过多级质谱信息得到精确的检测结果，层级递进的检索方式，不仅可以减少检索的工作量，还可以快速准确地检测出待检索色素的种类，减少筛查误差，最终实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
附图说明
为了更清楚地说明本申请实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本申请中记载的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本申请实施例一提供的合成色素的检测方法的流程图；
图2为本申请实施例二提供的合成色素的检测方法的流程图；
图3为本申请实施例三提供的合成色素的检测方法的流程图；
图4为本申请实施例四提供的合成色素的检测系统的结构示意图；
图5为本申请实施例五提供的合成色素的检测系统的结构示意图；
图6为本申请实施例六提供的合成色素的检测系统的结构示意图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例一：
图1为本申请实施例一提供的合成色素的检测方法的流程图。
参照图1所示，本申请实施例提供的合成色素的检测方法，用于检测食品样本中的待检索色素的种类，本申请实施例提供的合成色素的检测方法包括：
步骤S11：获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间。
在本申请实施例中，申请人可以通过研究近年来国内外期刊发表的合成色素类文章，以及现行在用的合成色素标准，对文献及标准中出现的色素进行归纳整理，预先建立的色素数据库。采用色素名称、检测方法、基体、检测限的 不同进行系统的标识和区分。通过文献及标准中合成色素的涉及频率，优先对高频色素进行建库，同样在色素数据库中以名称、CAS号、分子式、色指数等关键物化性质进行系统标识和区分。还可以在可能的物理化学性质参数中，确定一类参数和合成色素形成唯一对应关系，并以此在数据库中编号识别。比如对于绝大多数合成色素，均会有唯一的CAS号和色指数与之对应，并且CAS号及色指数这两个参数与分子式分子量等相比，具有清晰易查的优势。因此可以将这两个参数作为关键参数重点记录，提升色素数据库的检测应用便利程度。特别的，色指数作为合成色素一项物理参数，体现了色素在可见光区吸收特定波长区间的光后，产生特定的颜色这一特殊性质，在仪器检测方法的开发中，这一性质被利用的最多。此外，色素数据库还可以包括色素的常用中英文名称、分子式、分子量、分子结构、熔点、用途、主要来源等通用的物理化学性质信息。
在建立色素数据库后，在检测待检索色素时，可以通过仪器设备进行采集待检索色素的物化性质信息，然后输入到色素数据库中，就可以从数据库中得到相应的待检索区间。在通过待检索色素的物化性质信息进行检索时，可以通过中英文名称、CAS号、分子式、分子量、色指数等进行检索。比如，若待检索色素的碳数为20，则可在色素数据库中检索：C20，即可得到相应的待检索区间；或者若待检索色素的色指数(C.I.)为45430，则按照色指数检索即可得到待检索区间。
步骤S12：获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果。
在本申请实施例中，在确定待检索区间后，可以根据待检索色素的光谱信息从待检索区间中检索得到粗略检索结果。比如，若待检索色素在可见光区的吸收峰在530nm附近，则可以在待检索区间中进行检索得到粗略检索结果，进而达到缩小检索区间的目的，使得检索精度进一步提高。
在实际使用时，使用光谱仪器对色素进行分析时，波长范围设置为(200～700)nm，扫描速度采用120nm/min，狭缝宽度0.2nm。色素纯品称重后用溶剂(水/甲醇)配制成溶液，优先使用100％甲醇配制成溶液，部分合成色素不溶于甲醇时，采用100％水作为溶剂进行配制。通过具体实验发现，使用 水或者甲醇并不会给特征吸收峰数值带来变化，本申请优先使用甲醇，使数据库的应用更加广泛。溶液放入比色皿中进行扫描，在具体实验过程中通过适当调节溶液的浓度，合成色素的浓度在(5～40)×10-6范围内，使光谱数据中可见光区的特征吸收峰吸收值控制在(0.6～1.0)附近。
步骤S13：获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
在本申请实施例中，利用待检索色素的物化性质信息和光谱信息检索可以缩小检索范围，减少检索的工作量，当需要精确检索时，则可以使用待检索色素的多级质谱信息进行检索。比如，使用国家标准物质研制中心提供的赤藓红标准溶液模拟待检索色素，进行MS1-MS3的数据采集，并将多级质谱信息输入预先建立的色素数据库进行检索，通过具体实验发现，若待检索色素的一级质谱信息MS1进行检索，得到检索结果显示与某种色素的匹配度为65.78，进而以二级质谱信息MS2进行检索，得到检索结果显示与该种色素的匹配度为90.06，再以三级质谱信息MS3进行检索，得到检索结果显示与该种色素的匹配度为99.97。可以证明MS1信息受到基体环境、前处理不同匹配度不高，很难保证筛查的精确度，通过MS2、MS3的引入，使得筛查结果准确度得到保证，从而利用待检索色素的多级质谱信息在色素数据库中检索的非常必要，通过色素数据库储存的多级质谱信息，可以提高检索精度，减少对于待检索色素的定性误差。
在实际使用中，使用质谱仪器对色素进行分析时，仪器使用ESI源，在使用前经过全调谐优化，采用默认仪器参数设置，其中：CDL温度：200℃；Heat Block温度：200℃；干燥气流量:1.5L/min；检测电压:1.58kV；Interface电压(+):4.5kV；Interfce电压(-):-3.5kV；扫描范围：(100-1000)m/z。采用甲醇和水的缓冲盐溶液，当合成色素在质谱检测器上检出时，流动相中甲醇的比例一般在80％-100％，本申请优选采用0.1％甲酸-10mmol乙酸胺-水溶液和100％甲醇作为质谱仪流动相，比例为10：90。在此流动相下，各类合成色素均有良好响应。色素纯品称重后优先使用100％甲醇逐级稀释至10mg/L以下，进样量5μl。试样不经过色谱柱，直接进入质谱检测器进行分析。多级质谱误 差满足应用的要求，为精确定性待检索色素的种类提供了基础。
合成色素结构和性质的不同决定了质谱数据是以正离子模式还是负离子模式进行采集，在初步的数据采集工作中，所有待测色素都在两种模式下进行了扫描，选择离子响应最好的模式进行进一步的数据采集工作。
应用本申请提供的一种合成色素的检测方法，获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。这样，可以对现存已知的标准色素进行分析，根据得到的物化性质信息和谱图预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，缩小待检索色素在色素数据库中的检索范围，再通过多级质谱信息得到精确的检测结果，层级递进的检索方式，不仅可以减少检索的工作量，还可以快速准确地检测出待检索色素的种类，减少筛查误差，最终实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
实施例二：
图2为本申请实施例二提供的合成色素的检测方法的流程图。
参照图2所示，本申请实施例提供的合成色素的检测方法，用于检测食品样本中的待检索色素的种类，本申请实施例提供的合成色素的检测方法，在建立色素数据库时，包括如下步骤：
步骤S21：分析多种标准色素的物化性质信息，并根据所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库。
步骤S22：对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库。
步骤S23：对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库。
步骤S24：将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
在本申请实施例中，将获取的标准色素的物化性质信息、光谱信息、多级质谱信息导入ACD/Labs的数据库软件中，以色素为单位建立色素数据库。ACD/Labs将各部分信息结合成一个整体，每个色素的信息形成一个单元，每个单元都有色素的必要信息，如中英文名称、CAS号、色指数、分子式、分子结构、光谱信息、多级质谱信息等。
从而将待检索色素的物化性质信息、光谱信息、多级质谱信息输入建立完成的色素数据库后，就可以匹配搜索到色素数据库中的标准色素，即可得到待检索色素的种类。
应用本申请提供的一种合成色素的检测方法，获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。这样，可以对现存已知的标准色素进行分析，根据得到的物化性质信息和谱图预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，缩小待检索色素在色素数据库中的检索范围，再通过多级质谱信息得到精确的检测结果，层级递进的检索方式，不仅可以减少检索的工作量，还可以快速准确地检测出待检索色素的种类，减少筛查误差，最终实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
实施例三：
图3为本申请实施例三提供的合成色素的检测方法的流程图。
参照图3所示，本申请实施例提供的合成色素的检测方法，用于检测食品样本中的待检索色素的种类，包括如下步骤：
步骤S11：获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检 索色素的待检索区间。
步骤S12：获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果。
步骤S13：获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
步骤S14：根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
在本申请实施例中，当待检索色素的种类被确定后，色素数据库可以提供详细的该色素信息给检索者：包括名称、分子结构等物化信息，光谱图，多级质谱图、文献及标准等。这时，可以便利的进行快速筛查后的相关研究工作。例如通过质谱图检索确认赤藓红后，可以通过谱图处理软件和参考文献确定它的裂解途径，也可以找到与该色素相关的国内检测方法。这些工作能够对色素研究工作提供便利，对突发性食品安全事件起到快速响应的作用。
应用本申请提供的一种合成色素的检测方法，获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。这样，可以对现存已知的标准色素进行分析，根据得到的物化性质信息和光谱信息以及多级质谱信息预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，缩小待检索色素在色素数据库中的检索范围，再通过多级质谱信息得到精确的检测结果，层级递进的检索方式，不仅可以减少检索的工作量，还可以快速准确地检测出待检索色素的种类，减少筛查误差，最终实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
对于前述的各方法实施例，为了简单描述，故将其都表述为一系列的动作组合，但是本领域技术人员应该知悉，本发明并不受所描述的动作顺序的限制，因为依据本发明，某些步骤可以采用其他顺序或者同时进行。
本发明上述公开了合成色素的检测方法，相应的，本发明还公开了应用上述合成色素的检测方法的系统，该系统用于实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
实施例四：
图4为本申请实施例四提供的合成色素的检测系统的结构示意图。
参照图4所示，本申请实施例提供的合成色素的检测系统，用于检测食品样本中的待检索色素的种类，包括：
物化性质信息检测模块1，用于获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间。
在本申请实施例中，建立色素数据库可以使用ACD/Labs，该色素数据库通用于不同类型与不同原理的液相色谱串联质谱仪器的数据支持。该色素数据库所涉及的标准色素的来源可以是Chem Service公司和中国国家标准物质研制中心。标准色素的物化性质信息可以通过权威的化学文献检索获得。
光谱信息检测模块2，用于获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果。
在本申请实施例中，待检索色素的光谱信息可以由日立公司U-3900紫外可见光谱仪采集获取。
质谱信息检测模块3，用于获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
在本申请实施例中，待检索色素的多级质谱信息可以由岛津公司LCMS-IT-TOF离子捕获飞行时间质谱仪采集获取。与其他质谱仪相比，有着高精度、多级质谱、高检测速度等优势，这些特点均高度符合色素数据库应用需求，因此选用其作为质谱仪进行数据采集。
本申请实施例提供的电子设备，可以采用上述方法实施例中的信息传输方法，此处不再赘述。
实施例五：
图5为本申请实施例五提供的合成色素的检测系统的结构示意图。
参照图5所示，本申请实施例提供的合成色素的检测系统，用于检测食品样本中的待检索色素的种类，其中建立色素数据库的系统包括：
物化性质信息数据模块11，用于分析多种标准色素的物化性质信息，并根据所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库；
光谱信息数据模块12，用于对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库；
质谱信息数据模块13，用于对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库；
色素数据合并模块14，用于将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
本申请实施例提供的电子设备，可以采用上述方法实施例中的信息传输方法，此处不再赘述。
实施例六：
图6为本申请实施例六提供的合成色素的检测系统的结构示意图。
参照图6所示，本申请实施例提供的合成色素的检测系统，用于检测食品样本中的待检索色素的种类，包括：
物化性质信息检测模块1，用于获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间。
在本申请实施例中，建立色素数据库可以使用ACD/Labs，该色素数据库 通用于不同类型与不同原理的液相色谱串联质谱仪器的数据支持。该色素数据库所涉及的标准色素的来源可以是Chem Service公司和中国国家标准物质研制中心。标准色素的物化性质信息可以通过权威的化学文献检索获得。
光谱信息检测模块2，用于获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果。
在本申请实施例中，待检索色素的光谱信息可以由日立公司U-3900紫外可见光谱仪采集获取。
质谱信息检测模块3，用于获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
在本申请实施例中，待检索色素的多级质谱信息可以由岛津公司LCMS-IT-TOF离子捕获飞行时间质谱仪采集获取。与其他质谱仪相比，有着高精度、多级质谱、高检测速度等优势，这些特点均高度符合色素数据库应用需求，因此选用其作为质谱仪进行数据采集。
色素信息输出模块4，用于根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
本申请实施例提供的电子设备，可以采用上述方法实施例中的信息传输方法，此处不再赘述。
应用本申请提供的一种合成色素的检测方法及系统，获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。这样，可以对现存已知的标准色素进行分析，根据得到的物化性质信息和光谱信息以及多级质谱信息预先建立色素数据库，然后通过物化性质信息和光谱信息确定粗略的检索区间，缩小待检索色素在色素数 据库中的检索范围，再通过多级质谱信息得到精确的检测结果，层级递进的检索方式，不仅可以减少检索的工作量，还可以快速准确地检测出待检索色素的种类，减少筛查误差，最终实现对色素类别的快速准确检测，提高对突发食品安全事件的响应速度。
为了描述的方便，描述以上装置时以功能分为各种单元分别描述。当然，在实施本申请时可以把各单元的功能在同一个或多个软件和/或硬件中实现。
本说明书中的各个实施例均采用递进的方式描述，各个实施例之间相同相似的部分互相参见即可，每个实施例重点说明的都是与其他实施例的不同之处。尤其，对于装置或系统实施例而言，由于其基本相似于方法实施例，所以描述得比较简单，相关之处参见方法实施例的部分说明即可。以上所描述的装置及系统实施例仅仅是示意性的，其中所述作为分离部件说明的单元可以是或者也可以不是物理上分开的，作为单元显示的部件可以是或者也可以不是物理单元，即可以位于一个地方，或者也可以分布到多个网络单元上。可以根据实际的需要选择其中的部分或者全部模块来实现本实施例方案的目的。本领域普通技术人员在不付出创造性劳动的情况下，即可以理解并实施。
专业人员还可以进一步意识到，结合本文中所公开的实施例描述的各示例的单元及算法步骤，能够以电子硬件、计算机软件或者二者的结合来实现，为了清楚地说明硬件和软件的可互换性，在上述说明中已经按照功能一般性地描述了各示例的组成及步骤。这些功能究竟以硬件还是软件方式来执行，取决于技术方案的特定应用和设计约束条件。专业技术人员可以对每个特定的应用来使用不同方法来实现所描述的功能，但是这种实现不应认为超出本发明的范围。
结合本文中所公开的实施例描述的方法或算法的步骤可以直接用硬件、处理器执行的软件模块，或者二者的结合来实施。软件模块可以置于随机存储器(RAM)、内存、只读存储器(ROM)、电可编程ROM、电可擦除可编程ROM、寄存器、硬盘、可移动磁盘、CD-ROM、或技术领域内所公知的任意其它形式的存储介质中。
对所公开的实施例的上述说明，使本领域专业技术人员能够实现或使用本 发明。对这些实施例的多种修改对本领域的专业技术人员来说将是显而易见的，本文中所定义的一般原理可以在不脱离本发明的精神或范围的情况下，在其它实施例中实现。因此，本发明将不会被限制于本文所示的这些实施例，而是要符合与本文所公开的原理和新颖特点相一致的最宽的范围。

Claims (10)

  1. 一种合成色素的检测方法，其特征在于，用于检测食品样本中的待检索色素，包括：
    获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；
    获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；
    获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
  2. 根据权利要求1所述的合成色素的检测方法，其特征在于，所述物化性质信息，包括：色素名称、CAS号、分子式、分子量、分子结构和色指数。
  3. 根据权利要求1所述的合成色素的检测方法，其特征在于，所述色素数据库的建立方法包括：
    分析多种标准色素的物化性质信息，并根据所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库；
    对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库；
    对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库；
    将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
  4. 根据权利要求1所述的合成色素的检测方法，其特征在于，所述获取所述待检索色素的光谱信息，包括：
    以100％甲醇或100％水作为溶剂，配制所述待检索色素的溶液，使所述待检索色素的溶液浓度在(5～40)×10-6范围内；
    设置扫描所述待检索色素的波长范围为覆盖可见光区和紫外光区的 (200～700)nm，扫描速度为120nm/min，狭缝宽度为0.2nm；
    采集所述待检索色素的吸收波峰，并将所述吸收波峰作为所述待检索色素的光谱信息。
  5. 根据权利要求1所述的合成色素的检测方法，其特征在于，所述获取所述待检索色素的多级质谱信息，包括：
    以100％甲醇或100％水作为溶剂，配制所述待检索色素的溶液；
    以0.1％甲酸-10mmol乙酸胺-水溶液和100％甲醇作为流动相，且所述流动相中的甲醇的比例在80％-100％范围内；
    以(10-1000)m/z的扫描范围采集所述待检索色素的离子峰区间，作为所述待检索色素的光谱信息。
  6. 根据权利要求1所述的合成色素的检测方法，其特征在于，还包括：
    根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
  7. 一种合成色素的检测系统，其特征在于，用于检测食品样本中的待检索色素，包括：
    物化性质信息检测模块，用于获取所述食品样品中的待检索色素的至少一种物化性质信息，并根据所述至少一种物化性质信息，在预先建立的色素数据库中确定所述待检索色素的待检索区间；
    光谱信息检测模块，用于获取所述待检索色素的光谱信息，并根据所述光谱信息，在所述待检索区间中进行粗略检索，得到至少一个粗略检索结果；
    质谱信息检测模块，用于获取所述待检索色素的多级质谱信息，并根据所述多级质谱信息，在所述至少一个粗略检索结果中进行精确匹配，确定所述待检索色素的精确匹配结果。
  8. 根据权利要求7所述的合成色素的检测系统，其特征在于，所述物化性质信息，包括：色素名称、CAS号、分子式、分子量、分子结构和色指数。
  9. 根据权利要求7所述的合成色素的检测系统，其特征在于，所述预先建立的色素数据库，包括：
    物化性质信息数据模块，用于分析多种标准色素的物化性质信息，并根据 所述物化性质信息和对应的标准色素的映射关系建立物化性质信息数据库；
    光谱信息数据模块，用于对多种标准色素进行光谱扫描，采集多种标准色素的光谱信息，并根据所述光谱信息和对应的标准色素的映射关系建立光谱信息数据库；
    质谱信息数据模块，用于对多种标准色素进行质谱分析，得到多种标准色素的多级质谱信息，并根据所述多级质谱信息和对应的标准色素的映射关系建立多级质谱信息数据库；
    色素数据合并模块，用于将所述物化性质信息数据、所述光谱信息数据库和所述多级质谱信息数据库合并为所述色素数据库。
  10. 根据权利要求7所述的合成色素的检测系统，其特征在于，还包括：
    色素信息输出模块，用于根据所述待检索色素的精确匹配结果，输出所述待检索色素的色素信息；所述色素信息包括：色素名称、分子结构、光谱信息图、多级质谱信息图、参考检测标准、参考检测方法和参考文献。
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