CN115032315A - Method for detecting furfural in rice husk - Google Patents
Method for detecting furfural in rice husk Download PDFInfo
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Abstract
The application relates to the technical field of chaff detection, in particular to a method for detecting furfural in chaff, which comprises the following steps: (1) pulverizing and sieving testa oryzae to obtain testa oryzae powder; (2) adding an ethanol solution into the rice husk powder obtained in the step (1), oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%; (3) adding an extracting agent into the extracting solution obtained in the step (2) for oscillating extraction, and centrifuging to obtain an extracting solution; (4) filtering the extract, and detecting with gas chromatography-mass spectrometer. The method and the device can accurately detect the furfural in the chaff, and reduce the interference of other characteristic peaks on the characteristic peak of the furfural.
Description
Technical Field
The application relates to the technical field of chaff detection, in particular to a method for detecting furfural in chaff.
Background
The husk (rice hull) is an important auxiliary material for white spirit production, and is used as a filler and a loosening agent, and mainly plays roles of loosening, ventilation and water absorption. During the use of the husk in the brewing process, the higher the consumption of the husk is, the higher the furfural content in the wine body is, and the higher the furfural content is, so that the white wine can generate bran taste and dry spicy taste, thereby influencing the quality of the white wine. The development of the method for measuring the furfural in the rice husk is beneficial to monitoring the content of furfural in the rice husk potentially brought into the base wine from the source, and the quality control level of the white wine of an enterprise is further improved.
The existing detection method for furfural in chaff mainly carries out detection analysis through gas chromatography, and comprises the steps of steaming and crushing the chaff, then carrying out oscillation dissolution, carrying out ultrasonic extraction and filtration, and then entering a gas chromatograph for detection.
Due to the characteristic that the chaff is rich in the matrix of cellulose, lignin and silicon dioxide, the content of the chaff furfural is relatively low, and the furfural in the chaff cannot be accurately detected by the gas chromatography.
Disclosure of Invention
In order to detect furfural in the chaff more accurately, the application provides a method for detecting furfural in the chaff.
The application provides a detection method for furfural in chaff adopts the following technical scheme:
a method for detecting furfural in chaff comprises the following steps:
(1) pulverizing and sieving testa oryzae to obtain testa oryzae powder;
(2) adding an ethanol solution into the rice hull powder obtained in the step (1), oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%;
(3) adding an extracting agent into the extracting solution obtained in the step (2) for oscillating extraction, and centrifuging to obtain an extracting solution;
(4) filtering the extract, and detecting with gas chromatography-mass spectrometer.
Preferably, in the step (1), the grain husks are crushed and sieved, and the pore size is 0.5 mm.
Preferably, in the step (2), the ratio of the volume of the ethanol solution to the mass of the chaff powder is 4-10: 1; preferably, in the step (2), the ratio of the volume of the ethanol solution to the mass of the chaff powder is 6: 1.
Preferably, in the step (2), the oscillation time is 5-20 min, the centrifugation time is 5-7 min, and the centrifugation rotating speed is 5000-7000 r/min.
Preferably, in the step (2), the oscillation time is 15min, the centrifugation time is 6min, and the rotation speed of the centrifugation is 6000 r/min.
Preferably, the oscillation time of oscillation and centrifugation after the ethanol solution is added into the chaff sample is 15min, the centrifugation time is 6min, and the centrifugation speed is 6000 rpm/min.
Preferably, in the step (3), the extractant is diethyl ether.
Preferably, in the step (3), the time of the oscillating extraction is 1-10 min, the time of the centrifugation is 1-3 min, and the rotation speed of the centrifugation is 2000-3000 r/min; preferably, the time of the oscillation extraction is 1min, the time of the centrifugation is 2min, and the rotation speed of the centrifugation is 2500 r/min.
Preferably, in the step (4), the filtering the extract comprises: the filtration was carried out with a 0.22 μm filter.
Preferably, the gas chromatography parameters are set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 240-260 ℃, helium is used as carrier gas, the flow rate is 1-1.4 mL/min, and split-flow sample injection is not performed; temperature rising procedure: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is raised to 150 ℃ at the speed of 3-10 ℃/min, and then the temperature is raised to 230 ℃ at the speed of 15-25 ℃/min, and the temperature is kept for 10-12 min;
preferably, the gas chromatography parameters are set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 250 ℃, carrier gas is helium, the flow rate is 1.2mL/min, and split-flow sample injection is not carried out; temperature rising procedure: the initial temperature is 40 deg.C, and is maintained for 1min, then the temperature is raised to 150 deg.C at 5 deg.C/min, and then raised to 230 deg.C at 20 deg.C/min, and is maintained for 10 min.
The mass spectrum parameters are set as: selecting an EI ion source, wherein the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quadrupole rod temperature is 140-160 ℃, and the scanning mode is as follows: selecting an ion Scanning (SIM) mode;
preferably, the mass spectrum parameters are set as: selecting an EI ion source, wherein the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mode is as follows: an ion Scanning (SIM) mode is selected.
The application has the following beneficial technical effects:
according to the method, furfural in the chaff is extracted only through an ethanol solution in the pretreatment step, ultrasonic extraction is not needed, the pretreatment step is simplified, and the pretreatment time is shortened. In addition, the furfural in the rice husks is extracted by adopting an ethanol solution with the concentration of 20%, so that the extraction effect of the furfural in the rice husks is improved, the peak area of furfural detection can be improved, and the interference of other characteristic peaks on the characteristic peak of furfural is reduced; the accurate quantitative concentration of the detection method is ppb level, which is far lower than the accurate quantitative concentration of furfural in the chaff detected by gas chromatography in the prior art, which shows that the detection method can be used for detecting trace furfural or trace furfural in the chaff, and the detection result is more accurate and reliable.
Drawings
FIG. 1 is a comparison graph of furfural peak areas detected by sieving in crushing with different pore sizes in example 1 of the present application;
FIG. 2 is a comparison of furfural peak areas measured with different extraction solvents in example 2 of the present application;
FIG. 3 is a comparison graph of furfural peak areas measured for different ethanol solution concentrations in example 3 of the present application;
FIG. 4 is a comparison graph of furfural peak area measured for different ratios of ethanol solution volume to chaff powder mass in example 4 of the present application;
FIG. 5 is a comparison graph of furfural peak areas measured at different oscillation times in the ethanol solution extraction process in example 5 of the present application;
FIG. 6 is a comparison graph of furfural peak areas detected at different ultrasonic times in the ethanol solution extraction process in example 6 of the present application;
FIG. 7 is a comparison of furfural peak areas measured with different types of extractants during the extraction in example 7 of this application;
FIG. 8 is a comparison graph of furfural peak areas detected at different oscillation extraction times in the process of ether extraction in example 8 of the present application;
FIG. 9 is a gas chromatogram for the furfural detection method in the comparative example;
fig. 10 is a gas chromatography-mass spectrometry spectrum of the furfural detection method of the present application.
Detailed Description
At present, furfural (furfural) in chaff is detected mainly by a gas chromatograph, in the process of extracting furfural from chaff in pretreatment, an ethanol solution with the concentration of 50-60% needs to be adopted for extraction, and simultaneously, the mode of combining oscillation and ultrasound is also adopted for extraction, so that the furfural in the chaff can be extracted with a better extraction effect, the accuracy of detecting furfural in the chaff is improved, but the detection limit is higher, and when the content of furfural in the chaff is lower, the furfural in the chaff can not be accurately detected. The inventor finds that the furfural in the chaff can be accurately detected when the furfural in the chaff is detected by using a gas chromatography-mass spectrometer, and meanwhile, the detection result is not influenced by other characteristic peaks, and the detection concentration is low.
The present application is further illustrated by the following examples.
Reagent: acetone (with a concentration of more than or equal to 99.7%) and ether (with a concentration of more than or equal to 99.5%) were purchased from chemical reagents of national drug group, ltd; ethyl acetate (99.8% strength) was obtained from Merck, Germany; pentane (99.7% strength) was purchased from siemer feishel, usa.
The instrument comprises: gas chromatography-mass spectrometer, model: 7890B-5977B, available from Agilent, USA.
The application provides a detection method of furfural in chaff, which comprises the following steps:
(1) pulverizing testa oryzae, and sieving to obtain testa oryzae powder.
Specifically, the chaff is crushed and sieved by a cyclone sample mill to obtain chaff powder, the sieving aperture is 0.5mm, and 4g of the chaff powder is accurately weighed to be used as a sample to be detected for detection. The chaff in this application can be for not passing through the chaff of clear steaming, also can be for the chaff of clear after steaming, specifically select for not passing through the chaff of clear steaming in this application.
(2) And (2) adding an ethanol solution into the rice hull powder obtained in the step (1), oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%.
Specifically, 4g of chaff powder is added into a 50mL centrifuge tube, 24mL of 20% ethanol solution is added into the chaff powder, the mixture is oscillated for 15min at 450 times/min in a shaking table, then the mixture is centrifuged for 5-7 min, the centrifugation speed is 5000-7000 r/min, the centrifugation time is 6min, the centrifugation speed is 6000r/min, and the centrifuged supernatant is an extracting solution.
(3) And (3) adding an extracting agent into the extracting solution obtained in the step (2) for oscillating extraction, and centrifuging to obtain an extracting solution.
Specifically, 5mL of extracting solution is sucked and added into a 20mL sample bottle, 1.8g of NaCl is added, 1mL of diethyl ether is added as an extracting agent, vortex oscillation extraction is carried out for 1min, centrifugation is carried out for 1-3 min, the centrifugation rotating speed is 2000-3000 r/min, the centrifugation time is 2min, the centrifugation rotating speed is 2500r/min, and an upper organic phase is sucked after centrifugation to obtain the extracting solution.
(4) Filtering the extract, and detecting with gas chromatography-mass spectrometer.
Specifically, the extract was filtered through a 0.22 μm filter and used for gas chromatography-mass spectrometry (GC-MS) analysis.
The gas chromatography parameters in this application are set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 240-260 ℃, the carrier gas is helium, the flow rate is 1-1.4 mL/min, and split-flow sample injection is not performed; temperature rising procedure: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is raised to 150 ℃ at the speed of 3-10 ℃/min, and then the temperature is raised to 230 ℃ at the speed of 15-25 ℃/min, and the temperature is kept for 10-12 min; specifically, the gas chromatography parameters in this application are set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 250 ℃, carrier gas is helium, the flow rate is 1.2mL/min, and split-flow sample injection is not carried out; temperature rising procedure: the initial temperature is 40 deg.C, and is maintained for 1min, then the temperature is raised to 150 deg.C at 5 deg.C/min, and then raised to 230 deg.C at 20 deg.C/min, and is maintained for 10 min.
The mass spectrum parameters in this application are set as: selecting an EI ion source, wherein the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quadrupole rod temperature is 140-160 ℃, and the scanning mode is as follows: selecting an ion Scanning (SIM) mode; specifically, the mass spectrum parameters in the present application are set as: selecting an EI ion source, wherein the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mode is as follows: an ion Scanning (SIM) mode is selected.
Preparation of a standard solution: weighing a furfural standard substance, and preparing into ethanol solutions with the concentration of 20% respectively: 10.0 mu g/L, 20.0 mu g/L, 40.0 mu g/L, 80.0 mu g/L, 160.0 mu g/L, 320.0 mu g/L and 640.0 mu g/L of furfural standard solution. Detecting the furfural standard solution with different concentrations by adopting a gas chromatography-mass spectrometer according to the parameter setting, establishing a standard curve by taking the concentration of the furfural standard solution as a horizontal coordinate (X) and the corresponding peak area (Y) as a vertical coordinate, and obtaining a correlation coefficient (R) 2 ) The standard curve is 0.9987, the linearity of the standard curve is good, and the method can be used for quantitative detection of furfural.
Evaluation of the method
The precision of the furfural detection method in the rice husks is checked by Relative Standard Deviation (RSD), and the accuracy of the furfural detection method in the rice husks is verified by the standard recovery rate. Determination of relative standard deviation: and (3) detecting the furfural content in the samples for five times according to the furfural detection method in the chaff, and calculating the relative standard deviation, wherein the related detection results are shown in table 1. The RSD of the furfural determined by the method is 4.28%, which shows that the reproducibility of the detection method is good.
TABLE 1 relative standard deviation measurement results
| Sample (I) | Furfural content (μ g/kg) |
| |
147.8 |
| Chaff sample 2 | 158.9 |
| Chaff sample 3 | 156.8 |
| Chaff sample 4 | 146.0 |
| Chaff sample 5 | 145.1 |
| Relative Standard Deviation (RSD) | 4.28％ |
The recovery rate of the added standard is as follows: taking two parts of the same sample, adding a quantitative furfural standard substance into one part of the sample to obtain a standard sample, and simultaneously measuring the furfural content in the two parts of the sample by using the same detection method, wherein the ratio of the difference value between the measured value of the standard sample and the measured value of the non-standard sample to the amount of the added standard substance is the standard recovery rate of the sample. The calculation formula is as follows: the recovery on standard (measurement of the standard sample-measurement of the unlabeled sample) ÷ amount of standard substance added × 100%. The normalized recovery rate of the test method provided by the application is 87.59%, which shows that the method has high accuracy and can be used for detecting furfural in chaff.
The detection limit is determined according to the signal-to-noise ratio S/N which is more than or equal to 3, and the quantitative limit is determined according to the signal-to-noise ratio S/N which is more than or equal to 10. The detection limit of the detection method is 1.23 mug/kg, and the quantification limit is 4.09 mug/kg. The accurate quantitative concentration (the linear good concentration interval of the standard curve) of the detection method is ppb level, the accurate quantitative concentration of furfural in the chaff detected by adopting the gas chromatography in the prior art is ppm level, the accurate quantitative concentration of the detection method is far lower than the accurate quantitative concentration of furfural in the chaff detected by adopting the gas chromatography in the prior art, and the detection method can be used for detecting trace or trace furfural in the chaff, and the detection result is more accurate and reliable.
Example 1 investigation of the influence of the size of the pulverizing sieve on the assay results
In this embodiment, the method comprises the steps of grinding chaff by adopting cyclone samples with aperture of 0.5mm, 1.0mm and 2.0mm to obtain chaff powder, accurately weighing 4g of the chaff powder as chaff samples to be detected with three different particle sizes, and detecting the three kinds of chaff powder according to the following detection methods: putting the chaff sample into a 50mL centrifuge tube, adding 16mL of 40% ethanol solution as an extraction solvent, shaking for 15min by a shaker for 450 times/min, performing ultrasonic treatment for 5min, and centrifuging for 6min at a centrifugal rotating speed of 6000 r/min; sucking 5mL of supernatant into a 20mL sample bottle, adding 1.8g of NaCl, then adding 1mL of diethyl ether as an extracting agent, and performing vortex oscillation extraction for 1 min; centrifuging at 2500r/min for 2min for layering, and filtering the upper organic phase with 0.22 μm filter membrane for GC-MS analysis.
The gas chromatography parameters were set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 250 ℃, the carrier gas is helium, the flow rate is 1.2mL/min, and no shunt sample introduction is carried out; temperature rising procedure: the initial temperature is 40 deg.C, and is maintained for 1min, then the temperature is raised to 150 deg.C at 5 deg.C/min, and then raised to 230 deg.C at 20 deg.C/min, and is maintained for 10 min.
The mass spectrum parameters were set as: selecting an EI ion source, wherein the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mode is as follows: an ion Scanning (SIM) mode is selected.
The detection results of the crushed and sieved husk samples with three different pore sizes are shown in figure 1, and as can be seen from figure 1, when the husk is crushed by adopting a 0.5mm pore sieve, the furfural peak area is the largest, and the detection effect is the best. Both the 1.0mm and 2.0mm mesh screens, when used to crush chaff samples, reduce the instrumental response to detect furfural in the chaff. Therefore, select for use 0.5mm hole sieve to smash chaff in this application, carry out follow-up detection step again.
Example 2 investigation of the Effect of extraction solvent on assay results
In the present example, furfural in the husk powder was extracted with ethanol, acetone, ethyl acetate, and pentane as extraction solvents, and then the furfural was detected, and the rest of the detection steps were the same as those in example 1, and the husk was pulverized by using the 0.5 mm-mesh sieve preferable in example 1, and then the detection was performed.
The detection results of the four different extraction solvents are shown in fig. 2, and it can be seen from fig. 2 that when ethanol is selected as the extraction solvent, the peak area of furfural in the detected chaff is far larger than that of the other three extraction solvents, which indicates that ethanol is more suitable for being used as the extraction solvent to extract furfural in the chaff, and the other solvents are not suitable for extracting furfural in the chaff. Therefore, ethanol is chosen as the extraction solvent in the present application.
Example 3 investigation of the Effect of ethanol solution concentration on assay results
In this example, furfural in the husk powder was extracted with an ethanol solution (ultrapure water) having a concentration of 0%, an ethanol solution having a concentration of 10%, an ethanol solution having a concentration of 20%, an ethanol solution having a concentration of 30%, an ethanol solution having a concentration of 40%, and an ethanol solution having a concentration of 50% as extraction solvents, and then subjected to the examination, and the remaining examination procedures were the same as those in example 2.
The results of the detection of the ethanol solutions with six different concentrations as the extraction solvent are shown in fig. 3, and it can be seen from fig. 3 that the peak area detected by the ethanol solution with the concentration of 20% is the largest and far exceeds the peak area detected by the ethanol solutions with other concentrations. This shows that the 20% ethanol solution has a better extraction effect on furfural in the chaff, the detection result is more accurate, and the concentration of the rest ethanol solution is not suitable for extracting furfural in the chaff. Therefore, 20% ethanol solution was chosen as the extraction solvent in this application.
Example 4 the effect of the ratio of the volume of the ethanol solution to the mass of the chaff powder on the assay results was investigated
In this example, by fixing the weight of the husk powder to be 4g, different volumes of 20% ethanol solutions were added to change the ratio of the volume of the ethanol solution to the mass of the husk sample. The volume of ethanol solution comprises: 16mL (ratio of 4:1), 24mL (ratio of 6:1), 32mL (ratio of 8:1), 40mL (ratio of 10: 1). The remaining test procedures were the same as in example 3.
The results of the volume measurements of the four different ethanol solutions are shown in fig. 4, wherein the histogram is the furfural peak area measured according to the above ratio, and the column height represents the furfural peak area in 4g of husk powder, taking 16mL (ratio of 4:1) of ethanol solution as an example. As can be seen from the figure, as the ratio increases, the furfural peak area gradually decreases. The broken line in fig. 4 represents the area of furfural peak in a sample of rice husk extracted at 1g per 1mL of reagent. As can be seen from the figure, when the volume of the ethanol solution is 24mL, namely the ratio of the volume of the ethanol solution to the mass of the husk sample is 6:1, the area of the furfural peak extracted from 1g of the husk sample per 1mL of the reagent is the largest, and the extraction effect on furfural in the husk is the best. Thus, the volume of the ethanol solution in the present application was selected to be 24mL, when the ratio of the volume of the ethanol solution to the mass of the chaff sample was 6: 1.
Example 5 investigation of the influence of the shaking time on the assay results when ethanol solution was used to extract furfural from chaff
In the embodiment, in the process of extracting the furfural from the chaff by using the ethanol solution, the shaking is performed for 0min, 5min, 10min, 15min and 20min under the condition that the shaking table is used for 450 times/min, the rest detection steps are the same as those in the embodiment 4, the volume of the ethanol solution is selected to be 24mL, and the influence of different shaking time on the detection result is compared.
The detection results of different oscillation times in the five extraction processes are shown in fig. 5, and it can be seen from the figure that the oscillation time is within 0-15 min, the peak area of furfural is obviously increased along with the increase of the oscillation time, but the peak area of furfural is slightly increased within 15-20 min, and in order to improve the detection efficiency and reduce the energy consumption, the oscillation time in the extraction process is selected to be 15 min.
Example 6 investigation of the influence of ultrasound time on the test results
In the embodiment, in the process of extracting the furfural from the chaff by using the ethanol solution, after oscillating for 15min at 450 times/min by using a shaking table, ultrasonic treatment is respectively carried out for 0min (without ultrasonic treatment), 5min, 10min, 15min and 20min, the rest detection steps are the same as those in the embodiment 5, and the influence of different ultrasonic treatment time on the detection result is compared.
The detection results of different ultrasonic times in the five extraction processes are shown in fig. 6, and it can be seen from the figure that the furfural peak area has no obvious change from 0min to 20min along with the increase of the ultrasonic time, and the ultrasonic has no obvious effect on the extraction of the chaff furfural. Therefore, the extraction process in this application chooses not to sonicate.
Example 7 investigation of the Effect of different types of extractants on the assay results
In this example, the effect of different extractants on the detection result is compared, the addition amount of different kinds of extractions is 1mL, and the extractants include: diethyl ether, diethyl ether/pentane (diethyl ether and pentane mixed in a volume ratio of 1: 1), pentane, and the remaining detection steps were the same as in example 6.
The detection results of three different extractants are shown in fig. 7, and it can be seen from the figure that when diethyl ether is used as the extractant, the detected furfural peak area is the largest, which indicates that the diethyl ether has a better extraction effect. Therefore, diethyl ether is selected as the extraction solvent in this application.
Example 8 investigation of the Effect of the extraction time on the assay results
In this example, after 1mL of diethyl ether was added as an extractant, vortex extraction was performed for 0min, 1min, 3min, 5min, and 10min, and the remaining detection steps were the same as in example 7. And comparing the influence of different oscillation extraction time on the detection result in the extraction process.
The detection results of the five different oscillation extraction times are shown in fig. 8, and it can be seen from the figure that the vortex oscillation extraction time is within 0-1 min, and the furfural peak area also increases significantly with the increase of the vortex oscillation extraction time. The vortex oscillation extraction time is within 1-10 min, and the area of the furfural peak has no obvious change along with the increase of the vortex oscillation extraction time. Therefore, the time for vortex extraction in this application is chosen to be 1 min.
Comparative example
The method for detecting the furfural in the rice husks according to the existing gas chromatography specifically comprises the following steps: drying steamed chaff in an oven at 100-105 ℃ to constant weight, crushing the chaff, weighing and crushing 10.00g of oven-dried chaff with 40 meshes, putting the crushed chaff into a 100mL colorimetric tube, adding 50.0mL of 60% vol ethanol solution, oscillating and dissolving, carrying out ultrasonic extraction for 30min, and filtering to obtain a sample solution. Accurately sucking 5.00mL of sample solution and 0.50mL of internal standard solution to be uniformly mixed in a 10mL colorimetric tube. After the gas chromatograph is stabilized, 0.5 μ L of sample is injected for chromatographic analysis, and the detection result is shown in fig. 9. Fig. 10 is a chromatogram of a furfural standard product detected by GC-MS in the detection method of the present application, and as can be seen from fig. 9 and 10, furfural cannot be detected in chaff by the existing gas chromatography, and the furfural peak position is close to the peak of the acetic acid chromatogram, and furfural analysis is easily interfered by the peak of acetic acid. The detection method can be used for detecting the furfural in the chaff, the furfural is analyzed in a selective ion scanning mode of a gas chromatography-mass spectrometer, the chromatographic peak shape of the furfural is good, the interference of an acetic acid characteristic peak is removed, and the detection method has a lower quantitative limit, so that the detection result is clearer and more accurate.
According to the method, furfural in the rice husk is detected through a gas chromatography-mass spectrometer, the furfural in the rice husk is extracted through an ethanol solution with the concentration of 20% under the condition of not using ultrasonic waves, the furfural in the ethanol solution is extracted through an extracting agent, and finally the furfural is detected through the gas chromatography-mass spectrometer. According to the method, the furfural in the chaff is extracted by adopting the ethanol solution with the concentration of 20% under the condition of not using ultrasonic waves, and the furfural in the chaff can be accurately detected by adopting a gas chromatography-mass spectrometer, so that the interference of other characteristic peaks on the characteristic peak of the furfural is reduced.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. A detection method of furfural in chaff is characterized by comprising the following steps:
(1) pulverizing and sieving testa oryzae to obtain testa oryzae powder;
(2) adding an ethanol solution into the rice hull powder obtained in the step (1), oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%;
(3) adding an extracting agent into the extracting solution obtained in the step (2) for oscillating extraction, and centrifuging to obtain an extracting solution;
(4) filtering the extract, and detecting with gas chromatography-mass spectrometer.
2. The detection method according to claim 1, wherein in the step (1), the grain husks are crushed and sieved, and the pore size is 0.5 mm.
3. The detection method according to claim 1 or 2, wherein in the step (2), the ratio of the volume of the ethanol solution to the mass of the chaff powder is 4-10: 1; preferably, in the step (2), the ratio of the volume of the ethanol solution to the mass of the chaff powder is 6: 1.
4. The detection method according to claim 1 or 2, wherein in the step (2), the oscillation time is 5-20 min, the centrifugation time is 5-7 min, and the centrifugation rotation speed is 5000-7000 r/min.
5. The detection method according to claim 4, wherein in the step (2), the oscillation time is 15min, the centrifugation time is 6min, and the centrifugation rotation speed is 6000 r/min.
6. The detection method according to claim 1 or 2, wherein in the step (3), the extractant is diethyl ether.
7. The detection method according to claim 1 or 2, wherein in the step (3), the time of the shaking extraction is 1-10 min, the time of the centrifugation is 1-3 min, and the rotation speed of the centrifugation is 2000-3000 r/min; preferably, the time of the oscillating extraction is 1min, the time of the centrifugation is 2min, and the rotation speed of the centrifugation is 2500 r/min.
8. The detection method according to claim 1, wherein in the step (4), the filtering the extraction liquid comprises: the filtration was carried out with a 0.22 μm filter.
9. The detection method according to claim 1, wherein the gas chromatography parameters are set to: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 240-260 ℃, the carrier gas is helium, the flow rate is 1-1.4 mL/min, and split-flow sample injection is not performed; temperature rising procedure: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is raised to 150 ℃ at the speed of 3-10 ℃/min, and then the temperature is raised to 230 ℃ at the speed of 15-25 ℃/min, and the temperature is kept for 10-12 min;
preferably, the gas chromatography parameters are set as: the chromatographic column adopts DB-FFAP (30m multiplied by 0.25mm multiplied by 0.25 mu m) chromatographic column; the temperature of a sample inlet is 250 ℃, the carrier gas is helium, the flow rate is 1.2mL/min, and no shunt sample introduction is carried out; temperature rising procedure: the initial temperature is 40 deg.C, and is maintained for 1min, then the temperature is raised to 150 deg.C at 5 deg.C/min, and then raised to 230 deg.C at 20 deg.C/min, and is maintained for 10 min.
10. The detection method of claim 1, wherein the mass spectrometry parameters are set to: selecting an EI ion source, wherein the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quadrupole rod temperature is 140-160 ℃, and the scanning mode is as follows: selecting an ion Scanning (SIM) mode;
preferably, the mass spectrum parameters are set as: selecting an EI ion source, wherein the electron energy is 70eV, the ion source temperature is 230 ℃, the quadrupole rod temperature is 150 ℃, and the scanning mode is as follows: an ion Scan (SIM) mode is selected.
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| RU2265829C1 (en) * | 2004-07-19 | 2005-12-10 | Костромской государственный технологический университет | Method of determining content of free furfurol in plywood sized with furan resin |
| CN112858508A (en) * | 2021-01-13 | 2021-05-28 | 浙江省疾病预防控制中心 | Method for determining furfural compounds in coffee product |
| CN113009002A (en) * | 2019-12-20 | 2021-06-22 | 中粮营养健康研究院有限公司 | Sample pretreatment method containing furfural substances and method for detecting content of furfural substances |
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| RU2265829C1 (en) * | 2004-07-19 | 2005-12-10 | Костромской государственный технологический университет | Method of determining content of free furfurol in plywood sized with furan resin |
| CN113009002A (en) * | 2019-12-20 | 2021-06-22 | 中粮营养健康研究院有限公司 | Sample pretreatment method containing furfural substances and method for detecting content of furfural substances |
| CN112858508A (en) * | 2021-01-13 | 2021-05-28 | 浙江省疾病预防控制中心 | Method for determining furfural compounds in coffee product |
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