CN115032315B - Detection method of furfural in chaff - Google Patents
Detection method of furfural in chaff Download PDFInfo
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Abstract
The application relates to the technical field of chaff detection, in particular to a detection method of furfural in chaff, which comprises the following steps: (1) crushing and sieving chaff to obtain chaff powder; (2) Adding an ethanol solution into the rice husk powder obtained in the step (1), and then oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%; (3) Adding an extractant into the extract liquid obtained in the step (2) for oscillation extraction, and centrifuging to obtain an extract liquid; (4) The extract was filtered and then detected by a gas chromatograph-mass spectrometer. The application can accurately detect the furfural in the chaff and reduce the interference of other characteristic peaks on the characteristic peaks of the furfural.
Description
Technical Field
The application relates to the technical field of chaff detection, in particular to a detection method of furfural in chaff.
Background
Chaff (husk of rice) is an important auxiliary material for white spirit production, and is used as filler and bulking agent, and mainly has the functions of bulking, ventilation and water absorption. The husk contains poly pentose, which is hydrolyzed and then dehydrated and condensed to generate furfural, and the higher the husk consumption is, the higher the furfural content in the wine body is, the higher the furfural content can cause the wine to generate bran smell and dry spicy smell, thereby influencing the quality of the wine. The development of the measuring method of the chaff furfural is beneficial to monitoring the content of the chaff potentially brought into the base liquor furfural from the source, and further improves the quality control level of the white liquor of enterprises.
The existing detection method of furfural in chaff is mainly carried out by gas chromatography, and comprises the steps of steaming and crushing chaff, then carrying out oscillation dissolution, ultrasonic extraction and filtration, and then entering a gas chromatograph for detection.
Due to the matrix characteristics of the chaff rich in cellulose, lignin and silicon dioxide, the content of the chaff furfural is relatively low, and the gas chromatography method may not be capable of accurately detecting the furfural in the chaff.
Disclosure of Invention
In order to more accurately detect the furfural in the chaff, the application provides a detection method of the furfural in the chaff.
The detection method of furfural in chaff provided by the application adopts the following technical scheme:
a detection method of furfural in chaff comprises the following steps:
(1) Pulverizing testa oryzae, and sieving to obtain testa oryzae powder;
(2) Adding an ethanol solution into the rice husk powder obtained in the step (1), and then oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%;
(3) Adding an extractant into the extract liquid obtained in the step (2) for oscillation extraction, and centrifuging to obtain an extract liquid;
(4) The extract was filtered and then detected by a gas chromatograph-mass spectrometer.
Preferably, in the step (1), the aperture of the crushed and sieved chaff is 0.5mm.
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 husk powder is 6:1.
Preferably, in the step (2), the time of the oscillation is 5 to 20min, the time of the centrifugation is 5 to 7min, and the rotational speed of the centrifugation is 5000 to 7000r/min.
Preferably, in the step (2), the time of the oscillation is 15min, the time of the centrifugation is 6min, and the rotational speed of the centrifugation is 6000r/min.
Preferably, the shaking time of shaking and centrifuging after adding the ethanol solution to the chaff sample is 15min, the centrifuging time is 6min, and the centrifuging rotating speed is 6000rpm/min.
Preferably, in the step (3), the extractant is diethyl ether.
Preferably, in the step (3), the time of the oscillation extraction is 1-10 min, the time of the centrifugation is 1-3 min, and the rotating 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 rotating speed of the centrifugation is 2500r/min.
Preferably, in the step (4), the filtering the extract includes: filtration was performed using a filter membrane, which was a 0.22 μm filter membrane.
Preferably, the gas chromatography parameters are set as follows: the chromatographic column adopts DB-FFAP (30 m multiplied by 0.25mm multiplied by 0.25 μm) chromatographic column; the temperature of the sample inlet is 240-260 ℃, the carrier gas is helium, the flow rate is 1-1.4 mL/min, and sample injection is not split; heating program: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is increased to 150 ℃ at 3-10 ℃/min, then the temperature is increased to 230 ℃ at 15-25 ℃/min, and the temperature is kept for 10-12 min;
preferably, the gas chromatography parameters are set as follows: the chromatographic column adopts DB-FFAP (30 m multiplied by 0.25mm multiplied by 0.25 μm) chromatographic column; the temperature of the sample inlet is 250 ℃, the carrier gas is helium, the flow speed is 1.2mL/min, and sample injection is not split; heating program: the initial temperature was 40℃for 1min, then 5℃per min to 150℃and 20℃per min to 230℃for 10min.
The mass spectrum parameters are set as follows: an EI ion source is selected, the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quaternary rod temperature is 140-160 ℃, and the scanning mode is as follows: selecting an ion Scan (SIM) mode;
preferably, the mass spectrometry parameters are set as follows: an EI ion source is selected, the electron energy is 70eV, the ion source temperature is 230 ℃, the temperature of a four-level rod is 150 ℃, and the scanning mode is as follows: an ion Scan (SIM) mode is selected.
The application has the following beneficial technical effects:
in the pretreatment step, the furfural in the chaff is extracted only through the ethanol solution, ultrasonic extraction is not needed, the pretreatment step is simplified, and the pretreatment time is shortened. In addition, the furfural in the chaff is extracted by adopting the ethanol solution with the concentration of 20 percent, so that the extraction effect of the furfural in the chaff is improved, the peak area of furfural detection can be improved, and the interference of other characteristic peaks on the characteristic peaks of the furfural is reduced; the accurate quantitative concentration of the detection method is ppb level, which is far lower than that of the detection of furfural in chaff by adopting a gas chromatography method in the prior art, thus indicating that the detection method can be used for detecting trace or trace furfural in chaff, and the detection result is more accurate and reliable.
Drawings
FIG. 1 is a graph showing the comparison of the areas of furfural peaks detected by crushing and sieving with different apertures in example 1 of the present application;
FIG. 2 is a graph of the comparison of the areas of furfural peaks detected by different extraction solvents in example 2 of the present application;
FIG. 3 is a graph showing the comparison of the areas of furfural peaks detected by different ethanol solution concentrations in example 3 of the present application;
FIG. 4 is a plot of furfural peak area versus mass ratio of different ethanol solution volumes to chaff powder mass for example 4 of the present application;
FIG. 5 is a graph showing the comparison of the areas of furfural peaks detected at different oscillation times during the extraction of the ethanol solution according to example 5 of the present application;
FIG. 6 is a chart showing the comparison of the areas of furfural peaks detected at different ultrasonic times in the ethanol solution extraction process according to example 6 of the present application;
FIG. 7 is a graph showing the comparison of the areas of furfural peaks detected by different types of extractants during the extraction process in example 7 of the present application;
FIG. 8 is a graph showing the comparison of the areas of furfural peaks detected at different shaking extraction times during the diethyl ether extraction process according to example 8 of the present application;
FIG. 9 is a gas chromatogram of the furfural detection method in the comparative example;
fig. 10 is a gas chromatograph-mass spectrum in the furfural detection method of the present application.
Detailed Description
At present, the detection of furfural (furfural) in chaff is mainly carried out by adopting a gas chromatograph, in the process of extracting the furfural from the chaff by pretreatment, 50% -60% ethanol solution is required to be adopted for extraction, and meanwhile, a mode of combining oscillation and ultrasound is also required for extraction, so that the extraction effect of the furfural in the chaff is better, the accuracy of detecting the furfural in the chaff is improved, but the detection limit is higher, and when the content of the furfural in the chaff is lower, the furfural in the chaff possibly cannot be accurately detected. The inventor finds that when the gas chromatography-mass spectrometer is used for detecting the furfural in the chaff, the furfural in the chaff can be accurately detected, and meanwhile, the detection concentration is low, and other characteristic peaks do not influence the detection result.
The application is further illustrated by the following examples.
Reagent: acetone (concentration not less than 99.7%) and diethyl ether (concentration not less than 99.5%) were purchased from national pharmaceutical group chemical reagent company, ltd; ethyl acetate (concentration ∈99.8%) was purchased from merck, germany; pentane (99.7% strength) was purchased from sameimers, usa.
Instrument: gas chromatography-mass spectrometer, model: 7890B-5977B, available from Agilent corporation of America.
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 chaff powder is accurately weighed and used as a sample to be detected. The chaff in the application can be chaff which is not steamed, and can also be chaff which is steamed, and the chaff which is not steamed is specifically selected in the application.
(2) Adding an ethanol solution into the rice husk powder obtained in the step (1), and oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%.
Specifically, 4g of husk powder is added into a 50mL centrifuge tube, 24mL of ethanol solution with concentration of 20% is added into the husk powder, shaking is carried out for 15min under the condition of 450 times/min of a shaking table, and then the shaking table is centrifuged for 5-7 min at the rotational speed of 5000-7000 r/min.
(3) Adding an extractant into the extract liquid obtained in the step (2) for oscillation extraction, and centrifuging to obtain an extract liquid.
Specifically, 5mL of extracting solution is sucked and added into a 20mL sample bottle, then 1.8g of NaCl is added, then 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 speed is 2000-3000 r/min, the centrifugation time is selected to be 2min, the centrifugation speed is 2500r/min, and an upper organic phase is sucked after centrifugation, so that extracting solution is obtained.
(4) The extract was filtered and then detected by a gas chromatograph-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 the application are set as follows: the chromatographic column adopts DB-FFAP (30 m multiplied by 0.25mm multiplied by 0.25 μm) chromatographic column; the temperature of the sample inlet is 240-260 ℃, the carrier gas is helium, the flow rate is 1-1.4 mL/min, and sample injection is not split; heating program: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is increased to 150 ℃ at 3-10 ℃/min, then the temperature is increased to 230 ℃ at 15-25 ℃/min, and the temperature is kept for 10-12 min; specifically, the gas chromatography parameters in the application are set as follows: the chromatographic column adopts DB-FFAP (30 m multiplied by 0.25mm multiplied by 0.25 μm) chromatographic column; the temperature of the sample inlet is 250 ℃, the carrier gas is helium, the flow speed is 1.2mL/min, and sample injection is not split; heating program: the initial temperature was 40℃for 1min, then 5℃per min to 150℃and 20℃per min to 230℃for 10min.
The mass spectrum parameters in the application are set as follows: an EI ion source is selected, the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quaternary rod temperature is 140-160 ℃, and the scanning mode is as follows: selecting an ion Scan (SIM) mode; specifically, in the application, mass spectrum parameters are set as follows: an EI ion source is selected, the electron energy is 70eV, the ion source temperature is 230 ℃, the temperature of a four-level rod is 150 ℃, and the scanning mode is as follows: an ion Scan (SIM) mode is selected.
Preparing a standard solution: weighing a furfural standard substance, and respectively preparing the standard substance into a solution with 20% ethanol concentration: standard solutions of furfural of 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, 640.0. Mu.g/L. Detecting furfural standard solutions with different concentrations by adopting a gas chromatograph-mass spectrometer according to the parameter setting, establishing a standard curve by taking the concentration of the furfural standard solution as an abscissa (X) and the corresponding peak area (Y) as an ordinate, and correlatingCoefficient (R) 2 ) The standard curve has good linearity and can be used for quantitative detection of furfural, wherein the standard curve is 0.9987.
Method evaluation
The precision of the detection method of furfural in the chaff of the application is checked by Relative Standard Deviation (RSD), and the accuracy of the detection method of furfural in the chaff of the application is checked by the standard recovery rate. Determination of the relative standard deviation: the furfural content in the five samples was detected according to the above-mentioned method for detecting furfural in chaff, and then the relative standard deviation was calculated, and the results of the detection are shown in table 1. The RSD of the furfural measured by the method is 4.28%, which shows that the repeatability of the detection method is good.
Table 1 relative standard deviation measurement results
| Sample of | Furfural content (μg/kg) |
| Chaff sample 1 | 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 standard recovery rate is as follows: taking two identical samples, wherein one sample is added with quantitative furfural standard substance to obtain a labeled sample, the other sample is an unlabeled sample, then adopting the same detection method to simultaneously determine the quantity of furfural in the two samples, and obtaining the sample labeled recovery rate by the ratio of the difference value between the measured value of the labeled sample and the measured value of the unlabeled sample to the quantity of the added standard substance. The calculation formula is as follows: labeled recovery = (labeled sample measurement value-unlabeled sample measurement value)/(amount of added standard substance×100%). The labeling recovery rate of the test method provided by the application is 87.59%, the accuracy of the test method is high, and the method can be used for detecting furfural in chaff.
The application determines the detection limit according to the signal to noise ratio S/N more than or equal to 3, and determines the quantitative limit according to the signal to noise ratio S/N more than or equal to 10. The detection limit of the detection method was 1.23. Mu.g/kg, and the quantitative limit was 4.09. Mu.g/kg. The accurate quantitative concentration (the linear good concentration interval of the standard curve) of the detection method is ppb level, and the accurate quantitative concentration of the furfural in the chaff detected by adopting the gas chromatography in the prior art is ppm level, and the accurate quantitative concentration of the detection method is far lower than that of the furfural in the chaff detected by adopting the gas chromatography in the prior art, which indicates that 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 Effect of crushing sieving apertures on detection results
In the embodiment, cyclone samples with the pore diameters of 0.5mm, 1.0mm and 2.0mm are respectively adopted for grinding chaff to obtain chaff powder, 4g of chaff powder is respectively and accurately weighed as chaff samples to be detected with three different particle diameters, and the three chaff powders are respectively detected according to the following detection methods: putting a chaff sample into a 50mL centrifuge tube, adding 16mL of 40% ethanol solution as an extraction solvent, oscillating for 15min by a shaker 450 times/min, performing ultrasonic treatment for 5min, and centrifuging for 6min at a centrifugation 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 extractant, and carrying out vortex oscillation extraction for 1min; the mixture was centrifuged at 2500r/min for 2min for separation, and the upper organic phase was collected and filtered through a 0.22 μm filter membrane for GC-MS analysis.
The gas chromatography parameters were set as follows: the chromatographic column adopts DB-FFAP (30 m multiplied by 0.25mm multiplied by 0.25 μm) chromatographic column; the temperature of the sample inlet is 250 ℃, the carrier gas is helium, the flow speed is 1.2mL/min, and sample injection is not split; heating program: the initial temperature was 40℃for 1min, then 5℃per min to 150℃and 20℃per min to 230℃for 10min.
The mass spectrum parameters were set as: an EI ion source is selected, the electron energy is 70eV, the ion source temperature is 230 ℃, the temperature of a four-level rod is 150 ℃, and the scanning mode is as follows: an ion Scan (SIM) mode is selected.
The detection results of the chaff samples after crushing and sieving with three different apertures are shown in figure 1, and as can be seen from figure 1, when the chaff is crushed by adopting a 0.5 mm-aperture sieve, the peak area of furfural is the largest, and the detection effect is the best. When the chaff sample is crushed by adopting a 1.0 mm-hole sieve and a 2.0 mm-hole sieve, the response of an instrument for detecting furfural in chaff can be reduced. Therefore, in the application, the chaff is crushed by a sieve with 0.5mm holes, and then the subsequent detection step is carried out.
Example 2 investigation of the Effect of extraction solvent on detection results
In this example, the furfural in the husk powder was extracted with ethanol, acetone, ethyl acetate and pentane as extraction solvents, and then detected, and the other detection steps were the same as in example 1, and husk was crushed using the 0.5mm sieve preferable in example 1, and then detected.
The detection results of the four different extraction solvents are shown in fig. 2, and as can be seen from fig. 2, when ethanol is used 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 means that the ethanol is more suitable for extracting furfural in the chaff as the extraction solvent, and the rest solvents are not suitable for extracting furfural in the chaff. Thus, ethanol is selected as the extraction solvent in the present application.
Example 3 investigation of the Effect of ethanol solution concentration on detection results
In this example, furfural in chaff powder was extracted with 0% ethanol solution (ultrapure water), 10% ethanol solution, 20% ethanol solution, 30% ethanol solution, 40% ethanol solution, and 50% ethanol solution as extraction solvents, followed by detection, and the other detection steps were the same as in example 2.
The results of the detection of six different concentrations of ethanol solutions as extraction solvents are shown in fig. 3, and it can be seen from fig. 3 that the peak area detected is maximum when the concentration of the ethanol solution is 20%, and far exceeds the peak area detected with other concentrations of ethanol solutions. This shows that the 20% ethanol solution has better extraction effect on furfural in chaff, more accurate detection result and the concentration of the rest ethanol solution is not suitable for extracting furfural in chaff. Thus, an ethanol solution having a concentration of 20% was selected as the extraction solvent in the present application.
Example 4 investigation of the effect of the ratio of the volume of the ethanol solution to the mass of the chaff powder on the detection results
In the embodiment, the ratio of the volume of the ethanol solution to the mass of the husk sample is changed by fixing the mass of the husk powder to be constant and the mass to be 4g and adding different volumes of ethanol solutions with concentration of 20% respectively. The ethanol solution volume includes: 16mL (ratio of 4:1), 24mL (ratio of 6:1), 32mL (ratio of 8:1), 40mL (ratio of 10:1). The remaining detection steps were the same as in example 3.
The results of the detection of the four different ethanol solution volumes are shown in fig. 4, wherein the bar graph shows the furfural peak area detected according to the ratio, and the bar height shows the furfural peak area in 4g of husk powder by taking 16mL (the ratio is 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 furfural peak area per 1mL of reagent extraction in 1g of chaff sample. As can be seen from the figure, when the volume of the ethanol solution is 24mL, that is, the ratio of the volume of the ethanol solution to the mass of the chaff sample is 6:1, the area of the furfural peak in each 1mL of the reagent extracted from 1g of the chaff sample is the largest, and the extraction effect on the furfural in the chaff is the best. Thus, in the present application, the volume of the ethanol solution was selected to be 24mL, at which time the ratio of the volume of the ethanol solution to the mass of the chaff sample was 6:1.
Example 5 investigation of the Effect of the time of shaking on the detection results when extracting Furfural from chaff with ethanol solution
In the embodiment, in extracting the chaff furfural by using the ethanol solution, shaking for 0min, 5min, 10min, 15min and 20min respectively under the condition of shaking table 450 times/min, the rest detection steps are the same as those of 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 graph that the oscillation time is within 0-15 min, the peak area of furfural increases obviously along with the increase of the oscillation time, but the increase of the peak area of furfural is less within 15-20 min, so that the oscillation time in the extraction process is selected to be 15min for improving the detection efficiency and reducing the energy consumption.
Example 6 investigation of the Effect of ultrasound time on detection results
In the embodiment, in extracting the chaff furfural by using the ethanol solution, after shaking for 15min at the speed of 450 times/min on a shaking table, respectively performing ultrasonic treatment for 0min (without ultrasonic treatment), 5min, 10min, 15min and 20min, and comparing the influence of different ultrasonic time on the detection result by other detection steps in the same way as in the embodiment 5.
The detection results of different ultrasonic times in the five extraction processes are shown in fig. 6, and from the graph, it can be seen that the peak area of the furfural is not obviously changed along with the increase of the ultrasonic time from 0min to 20min, and the ultrasonic has no obvious effect on extracting the chaff furfural. Therefore, the extraction process in the present application chooses not to be ultrasonic.
Example 7 investigation of the Effect of different kinds of extractants on detection results
In this embodiment, the influence of different extractants on the detection result is compared, the addition amounts of different types of extraction are all 1mL, and the extractants include: diethyl ether, diethyl ether/pentane (diethyl ether and pentane mixed in a volume ratio of 1:1), pentane, the remaining detection steps were the same as in example 6.
The detection results of the three different extractants are shown in fig. 7, and it can be seen from the graph that when diethyl ether is used as the extractant, the detected furfural peak area is the largest, which indicates that the diethyl ether has better extraction effect. Therefore, diethyl ether is selected as the extraction solvent in the present application.
Example 8 investigation of the Effect of the time of shaking extraction on the detection results during diethyl ether extraction
In this example, after 1mL of diethyl ether was added as an extractant, the extraction was performed for 0min, 1min, 3min, 5min, and 10min with vortexing, respectively, 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 graph that the vortex oscillation extraction time is within 0-1 min, and along with the increase of the vortex oscillation extraction time, the furfural peak area is also obviously increased. The vortex oscillation extraction time is within 1-10 min, and the furfural peak area is not obviously changed along with the increase of the vortex oscillation extraction time. Therefore, the time of vortex extraction in the present application was chosen to be 1min.
Comparative example
Detecting furfural in chaff according to the existing gas chromatography, specifically comprising the following steps: drying steamed chaff to constant weight in a baking oven at 100-105 ℃, crushing the chaff, weighing 10.00g of absolute dried chaff crushed to 40 meshes, placing the dried chaff into a 100mL colorimetric tube, adding 50.0mL of 60% vol ethanol solution, oscillating for dissolving, ultrasonically extracting for 30min, and filtering to obtain a sample solution. Accurately sucking 5.00mL of sample solution, and uniformly mixing 0.50mL of internal standard solution in a 10mL colorimetric tube. After the gas chromatograph was stabilized, 0.5. Mu.L of sample was introduced for chromatographic analysis, and the detection result was shown in FIG. 9. Fig. 10 is a chromatogram of a standard furfural sample detected by GC-MS in the detection method of the present application, and as can be seen from fig. 9 and 10, the existing gas chromatography fails to detect furfural in chaff, and the peak position of furfural is close to the acetic acid chromatographic peak, and the analysis of furfural is easily interfered by the acetic acid peak. The detection method can be used for detecting the furfural in the chaff, the furfural is analyzed by a selective ion scanning mode of a gas chromatography-mass spectrometer, the chromatographic peak shape of the furfural is good, the interference of the characteristic peak of acetic acid is removed, and the detection method has lower quantitative limit, so that the detection result is clearer and more accurate.
According to the application, furfural in chaff is detected by a gas chromatography-mass spectrometer, the furfural in chaff is extracted by an ethanol solution with the concentration of 20% under the condition of not using ultrasound, then the furfural in the ethanol solution is extracted by an extractant, and finally the detection is performed by the gas chromatography-mass spectrometer. According to the application, the furfural in the chaff is extracted by adopting the ethanol solution with the concentration of 20% under the condition of not using ultrasound, and is detected by adopting the gas chromatography-mass spectrometer, so that the furfural in the chaff can be accurately detected, and the interference of other characteristic peaks on the characteristic peaks of the furfural is reduced.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (12)
1. The detection method of the furfural in the chaff is characterized by comprising the following steps of:
(1) Pulverizing testa oryzae, and sieving to obtain testa oryzae powder;
(2) Adding an ethanol solution into the rice husk powder obtained in the step (1), and then oscillating and centrifuging to obtain an extracting solution, wherein the concentration of the ethanol solution is 20%, and the ratio of the volume of the ethanol solution to the mass of the rice husk powder is 4-10:1;
(3) Adding an extractant into the extracting solution obtained in the step (2) for oscillation extraction, and centrifuging to obtain an extracting solution, wherein the extractant is diethyl ether;
(4) Filtering the extract, and detecting by using a gas chromatograph-mass spectrometer; wherein, the chromatographic column adopts DB-FFAP chromatographic column with specification of 30m multiplied by 0.25mm multiplied by 0.25 μm; heating program: the initial temperature is 35-45 ℃, the temperature is kept for 1-2 min, then the temperature is increased to 150 ℃ at 3-10 ℃/min, and then the temperature is increased to 230 ℃ at 15-25 ℃/min, and the temperature is kept for 10-12 min.
2. The method according to claim 1, wherein in the step (1), the size of the particle size of the chaff is 0.5mm.
3. The 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 6:1.
4. The method according to claim 1 or 2, wherein in the step (2), the time of the shaking is 5 to 20min, the time of the centrifugation is 5 to 7min, and the rotational speed of the centrifugation is 5000 to 7000r/min.
5. The method according to claim 4, wherein in the step (2), the time of the shaking is 15min, the time of the centrifugation is 6min, and the rotational speed of the centrifugation is 6000r/min.
6. The method according to claim 1 or 2, wherein in the step (3), the time of the shaking extraction is 1 to 10min, the time of the centrifugation is 1 to 3min, and the rotational speed of the centrifugation is 2000 to 3000r/min.
7. The method according to claim 1 or 2, wherein in the step (3), the time of the shaking extraction is 1min, the time of the centrifugation is 2min, and the rotational speed of the centrifugation is 2500r/min.
8. The method according to claim 1, wherein in the step (4), the filtering the extract liquid comprises: filtration was performed using a filter membrane, which was a 0.22 μm filter membrane.
9. The method according to claim 1, wherein the gas chromatography parameter is set as: the temperature of the sample inlet is 240-260 ℃, the carrier gas is helium, the flow rate is 1-1.4 mL/min, and the sample is not split.
10. The method according to claim 1, wherein the gas chromatography parameter is set as: the temperature of the sample inlet is 250 ℃, the carrier gas is helium, the flow speed is 1.2mL/min, and sample injection is not split; heating program: the initial temperature was 40℃for 1min, then 5℃per min to 150℃and 20℃per min to 230℃for 10min.
11. The method of claim 1, wherein the mass spectrometry parameters are set to: an EI ion source is selected, the electron energy is 65-75 eV, the ion source temperature is 220-240 ℃, the quaternary rod temperature is 140-160 ℃, and the scanning mode is as follows: an ion scan mode is selected.
12. The method of claim 1, wherein the mass spectrometry parameters are set to: an EI ion source is selected, the electron energy is 70eV, the ion source temperature is 230 ℃, the temperature of a four-level rod is 150 ℃, and the scanning mode is as follows: an ion scan mode is selected.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 陈锦屏 等.不同升温方式对烘干枣品质影响的研究.农业工程学报.1999,第15卷237-240. * |
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