CN112505223B - Method for simultaneously detecting content of toxoflavin and content of mirostrobin in food - Google Patents
Method for simultaneously detecting content of toxoflavin and content of mirostrobin in food Download PDFInfo
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- CN112505223B CN112505223B CN202011354358.6A CN202011354358A CN112505223B CN 112505223 B CN112505223 B CN 112505223B CN 202011354358 A CN202011354358 A CN 202011354358A CN 112505223 B CN112505223 B CN 112505223B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Abstract
The invention provides a simple and efficient method for simultaneously detecting the contents of toxoflavin and fermentation starter acid in food, which comprises the following steps: 1) Pretreating a sample, extracting the sample twice, vortexing the sample by using 80-90% methanol aqueous solution, performing ultrasonic treatment, then centrifuging the sample, sucking supernatant liquid into a centrifugal tube pre-filled with dSPE EMR-Lipid adsorbent, vortexing and centrifuging the supernatant liquid, and taking the supernatant liquid; mixing the supernatants, performing nitrogen blowing treatment on the obtained supernatant, diluting to constant volume with methanol, and filtering with a filter membrane; 2) Carrying out chromatographic analysis on the treated sample obtained in the step 1), wherein the chromatographic conditions comprise: the chromatographic column is a C18 chromatographic column; the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is methanol, and the mobile phase B is water with the pH value of 2.5-3.0; 3) Quantitatively analyzing the content of toxoflavin and fermentation broth acid in the sample.
Description
Technical Field
The invention relates to a quantitative analysis and detection technology of toxoflavin and mirinomycelic acid, in particular to a method for simultaneously detecting the contents of toxoflavin and mirinomycelic acid in food.
Background
In recent years, food poisoning events caused by Pseudomonas coevensis subsp.farinofaciens (Pseudomonas coevensis subsp.farinofacienans, pseudomonas coenospora for short) occur occasionally, and relate to food types including cereal fermentation products, deteriorated tremella, potato products and the like. Under the conditions of proper temperature, humidity and the like, pseudomonas cocoanut produces two toxins, namely mirinogenic acid (BA) and Toxoflavin (TF). Toxicology studies have shown that the LD50 of BA for mouse intravenous injection is 1.14mg/kg, the MED50 is 0.0562mg/kg, the LD50 of TF for mouse intravenous injection is 1.7mg/kg, and the MED50 is 8.39mg/kg, wherein, the fermentation broth is heat-resistant, and the general cooking method can not remove, which is also one of the main reasons of high fatality rate caused by food poisoning caused by pseudomonas cocoanulata.
At present, aiming at the investigation of food poisoning events caused by pseudomonas cocofermentum, pathogenic bacteria separation and identification and toxin determination work are mainly carried out. The separation and identification of pathogenic bacteria of the coconut toxin pseudomonas fermented rice flour subspecies can refer to GB/T4789.29-2003 'food hygiene microbiology inspection of coconut toxin pseudomonas fermented rice flour subspecies inspection', the content measurement of toxin fermentation mycolic acid refers to GB 5009.189-2016 'determination of fermentation mycolic acid in food safety national standard food', and toxoflavin has no national standard method temporarily. Suzuki et al (Suzuki F, sawada H, azegami K, et al. Molecular characterization of the toxopan-induced in toxoflavin biosynthesis of Burkholderia glumae. J Gen Plant Pathol,2004, 70) and Zhu et al (Suzuki F, sawada H, azegami K, et al. Molecular characterization of the toxopan-induced in toxoflavin biosynthesis of Burkholderia glumae. J Gen Plant Pathol,2004, 70) were qualitatively analyzed by thin layer chromatography; buckle KA (Buckle KA, kartagarma E.inhibition of bongkrek acid and toxoflavin production in tempore bongkrek containment microorganisms. J Appl Bacteriol,1990, 68) and Fenwick MK (Fenwick MK, philmus B, begley TP, et al. Toxoflavin lyase hydrolysis a novel 1-His-2-carboxylate surfactant project. Biochemistry,2011, 50) developed HPLC mass spectrometry and liquid chromatography mass spectrometry, respectively, to determine the concentration of flavin in a culture solution, although the applicable test ranges are narrow; in recent years, plum blossom is bright; zhangdonley et al (plum red color; zhangdonley; shenghua, etc.. Studies on the detection method of bacterial toxin of mirianic acid and toxoflavin in complex food matrix based on solid phase extraction-high performance liquid chromatography [ Z ] national scientific achievements, plum red color, swiftlet fly, huanghaizhi, etc.. High performance liquid chromatography-diode array detector combined with solid phase extraction method to rapidly determine mirianoic acid residue [ J ] in food, food science, 2016,37 (24): 254-258.) developed the detection method of bacterial toxin of mirianic acid and toxoflavin in complex food matrix based on solid phase extraction-high performance liquid chromatography by respectively purifying mirianoic acid and toxoflavin with mixed weak anion small column (WAX) and multifunctional purification column MycoSep 226, and then combining and concentrating for determination, but the method has complicated operation steps, large loss of organic solvent, and long concentration time for food with large starch content such as rice and flour products. There is a need to develop a rapid purification method, shorten the pretreatment time, and realize the method for simultaneously detecting the contents of toxoflavin and fermentation broth, so as to improve the detection and analysis efficiency of toxoflavin and fermentation broth in food.
Disclosure of Invention
The invention aims to provide a simple and efficient method for simultaneously detecting the contents of toxoflavin and mirostrobin.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides a method for simultaneously detecting the content of flavochrome and miroectose in food, which comprises the following steps:
1) Pretreating a sample
Extracting the sample twice, vortexing 80-90% (volume percent) methanol aqueous solution for 2-5min, performing ultrasonic treatment for 10-15min, centrifuging, sucking the supernatant into a centrifuge tube pre-filled with dSPE EMR-Lipid adsorbent (the amount of the adsorbent is the preset amount of the adsorbent commodity), vortexing for 2-5min, centrifuging, and taking the supernatant;
mixing the supernatants obtained by the two extractions, performing nitrogen blowing treatment on the obtained supernatant, performing constant volume with methanol, and filtering with a filter membrane to obtain a treated sample;
2) Carrying out chromatographic analysis on the treated sample obtained in the step 1), wherein the chromatographic conditions comprise: the chromatographic column is a C18 chromatographic column; the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is methanol, and the mobile phase B is water with the pH value of 2.5-3.0; the detection wavelength is 258nm; the gradient elution procedure was:
0-5min, 20% of mobile phase A and 80% of mobile phase B;
5-6min, mobile phase A20% → 90%, mobile phase B80% → 10%;
6-14min, mobile phase A90%, mobile phase B10%;
14-15min, mobile phase A90% → 20%, mobile phase B10% → 80%;
15-20min, mobile phase A20%, mobile phase B80%;
the above percentages all refer to volume percentages in the mobile phase;
3) And (3) quantitatively analyzing the content of the flavonol and the mirinomycin acid in the sample according to a pre-drawn standard curve and the detection result (such as a response peak area obtained by chromatographic analysis) obtained by chromatographic analysis in the step 2).
In a preferred embodiment, the pH of the water as mobile phase B in step 2) is 3.0.
In a preferred embodiment, in step 2), formic acid is used as the water of the mobile phase B to adjust the pH to 3.0.
In a preferred embodiment, in step 1), the concentration of the aqueous methanol solution is 80%.
In some embodiments, the aqueous methanol solution is used in an amount of 10ml per 2g of sample in step 1).
In some embodiments, in step 2), the chromatographic conditions further comprise: the flow rate is 1mL/min; the column temperature is 30 ℃; the amount of sample was 10. Mu.L.
The food samples used in the detection method of the invention can be various food samples required for detecting the content of toxoflavin and fermentation rice acids, such as but not limited to cereal fermentation products, potato products, tremella and/or black fungus, for example corn flour, wet rice noodles and the like.
Specifically, the present invention employs an external standard method for the quantitative analysis.
The technical scheme provided by the invention has the following beneficial effects:
the method provided by the invention can be used for simply, quickly and highly sensitively detecting the contents of the flavonol and the rice ferment acid in the food, simplifying the detection process and improving the detection efficiency.
Drawings
FIG. 1 is a graph of the effect of different extraction solvents on recovery of toxoflavin and mirinomycelic acid;
FIG. 2 is a graph showing the effect of different concentrations of methanol solutions on recovery of toxoflavin and mirinomycelic acid;
FIG. 3 is a graph showing the effect of different extraction times on recovery of toxoflavin and mirinomycelic acid using 80% methanol as a solvent;
FIGS. 4-1 and 4-2 are respectively spectra of toxoflavin and mirinomycesic acid in sequence;
FIG. 5 is a chromatogram of different mobile phase acidity regulators;
figure 6 is a mobile phase chromatogram at different pH.
Detailed Description
In order to better understand the technical solution of the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
In the following examples or comparative examples, the apparatus, materials and reagents used are as follows:
an experimental instrument:
agilent 1260 high performance liquid chromatograph with DAD detector (Agilent 4212A 1260, agilent, inc.); GT-2227QTS Intelligent ultrasonic cleaner (Guangdong ultrasound Co., ltd.); the Foctor Plus high-throughput fully automatic solid phase extraction instrument (Xiameni Rui group, inc.).
Materials and reagents:
toxoflavin (CAS number: 84-82-2, purity is not less than 98%), fermentation starter acid (CAS number: 11076-19-0, purity is not less than 95%), methanol and acetonitrile are in chromatographic purity, quEChERS dSPE EMR-Lipid (Anguilentechnology, inc., guangzhou), polish Tube-NaCl/MgSO 4 (Agilent technologies, inc., guangzhou), dSPE Cleaneuup Tubes (300 mg MgSO. RTM.) 4 100mg PSA,100mg C18, 15mL) (Shanghai spectral laboratory science and technology Co., ltd.), cleanert MAS-Q (PSA 400mg, C18 400mg, mgSO 4) 4 1.2g, 15mL) (Tianjin Bonnaijier science, ltd.); the other reagents are analytically pure; the experimental water was ultrapure water.
Preparation of standard solution for drawing standard curve:
milomycetic acid standard stock solution (0.1 mg/mL): 1mg (accurate to 0.01 mg) of the fermentation starter acid standard substance is accurately weighed, dissolved by methanol, transferred to a 10mL volumetric flask and subjected to constant volume by methanol.
Toxoflavin standard stock (0.1 mg/mL): 1mg (accurate to 0.01 mg) of toxoflavin standard substance is accurately weighed, dissolved by methanol, transferred to a 10mL volumetric flask and added with methanol to a constant volume.
Linear relationships, method detection limits and quantitation limits:
the method comprises the steps of respectively taking the standard stock solution of the mirermentacid and the standard stock solution of the toxoflavin as stock solutions, and sequentially and respectively preparing series of standard solutions with the concentrations of 0.5, 1.0, 2.0, 5.0, 10.0 and 25.0 mu g/mL. The analysis was performed under the same chromatographic conditions as in example 1 below, and the peak area of the standard solution was determined. Taking the peak area as an ordinate and the toxoflavin and the mircotoxiconazole concentration as an abscissa, a standard curve is drawn, and the linear relation, the detection limit of the method and the quantitative limit are shown in table 1. The result shows that toxoflavin and the fermentation broth acid present good linear relation in the range of 0.5-25 mug/ml.
Chromatographic conditions are as follows: chromatographic column C 18 A chromatographic column (column length 250mm, inner diameter 4.6mm, particle size 5 μm); the mobile phase A is methanol, and B is water (the pH value is adjusted to 3.0 by formic acid); flow rate: 1mL/min; detection wavelength: 258nm; column temperature: 30 ℃; sample injection amount: 10 μ L, gradient elution procedure see Table 2 in example 1.
TABLE 1 Linear relationship of mirinomycins and toxoflavins, method detection limits and quantitation limits
Example 1
1.1 detection method
Sample pretreatment: weighing 2g (accurate to 0.01 g) of the crushed/uniformly mixed sample into a 50mL plastic centrifuge tube, adding 10mL of 80% methanol aqueous solution (used as an extraction solvent), carrying out vortex for 2min, carrying out ultrasonic 10min, carrying out centrifugation for 5min at 5000r/min, sucking supernatant into the centrifuge tube filled with dSPE EMR-Lipid adsorbent (the dosage is the preset dosage of a commodity), carrying out vortex for 2min, carrying out centrifugation for 5min at 5000r/min, and taking the supernatant into a nitrogen blowpipe; meanwhile, the extraction and purification steps are repeated, the two supernatants are combined and blown to less than 1ml in water bath at 40 ℃, methanol is used for fixing the volume to 1ml, and chromatographic analysis is carried out after filtering by a 0.22 mu m filter membrane.
Chromatographic conditions are as follows: chromatographic column C 18 A chromatography column (column length 250mm, inner diameter 4.6mm, particle size 5 μm); the mobile phase A is methanol, and the mobile phase B is water (the pH is adjusted to 3.0 by formic acid); flow rate: 1mL/min; detection wavelength: 258nm; column temperature: 30 ℃; sample introduction amount: 10 μ L, gradient elution program see Table 2.
And quantifying by an external standard method, and calculating to obtain the content of toxoflavin and the content of the fermentation broth acid in the sample according to a drawn standard curve and a chromatographic detection result.
Table 2 gradient elution procedure (the following percentages are by volume)
1.2 stability test of detection method
According to the detection method of the embodiment 1, wet rice flour is used as a sample, the prepared test solution is placed at room temperature, and is respectively measured once after being placed for 0 hour, 6 hours, 12 hours, 18 hours, 24 hours and 30 hours, the total number of the measurements is 6, the RSD of the toxoflavin peak area within 18 hours is 4.79 percent, the RSD is obviously attenuated, and the RSD is far more than 5 percent; the RSD of the peak area of the miroavulanic acid in 36h is 0.83%, and the stability is good.
1.3 method recovery and precision
And (3) sample standard addition recovery rate: taking two parts of the same sample, and adding a quantitative standard substance of the component to be detected into one part of the sample; and (3) simultaneously analyzing the two parts according to the same analysis step, subtracting the result obtained by adding the part without the standard from the result obtained by adding the part with the standard, and determining the ratio of the difference value to the theoretical value of the added standard substance as the sample standard adding recovery rate.
Standard recovery = (standard sample measurement value-sample measurement value) ÷ standard addition × 100%
According to the detection method of example 1, 4 different matrixes of tremella, black fungus, corn flour and wet rice flour are selected to perform 3-level addition recovery rate (standard recovery rate) experiments and precision experiments, and the result (table 3) shows that under 2ug/mL, 8ug/mL and 16ug/mL of 3 standard addition levels, the average recovery rate (n = 6) of toxoflavin is 88.94%, and the average relative standard deviation (RSD, n = 6) is 1.50%; the mean recovery of mirinogenic acid (n = 6) was 90.43%, the mean relative standard deviation (RSD, n = 6) was 1.43%; the method has good accuracy and precision.
TABLE 3 recovery of toxoflavin and mirinoac results (n = 6)
Example 2
The detection method of this example is substantially the same as that of example 1, except that wet rice flour is used as a sample, and methanol, acetonitrile, 80% methanol, and 80% acetonitrile are used as extraction solvents in the sample pretreatment, and the results of comparing the recovery rates of toxoflavin and mirinocenic acid using these four different solvents are shown in fig. 1.
As can be seen from FIG. 1, the extraction effect of 80% methanol aqueous solution is better than that of methanol, acetonitrile and 80% acetonitrile, and the recovery rates of toxoflavin and mirostrobin are respectively 95.3% and 87.1%.
Example 3
The difference between the test methods of this example and example 1 is that wet rice flour is used as a sample, and in the sample pretreatment, 60% methanol aqueous solution, 70% methanol aqueous solution, 80% methanol aqueous solution, 90% methanol aqueous solution and 100% methanol are used as extraction solvents, and the results of comparison of recovery rates using these four methanol solutions with different concentrations are shown in fig. 2. As can be seen from FIG. 2, when 80% methanol is selected, recovery rates of toxoflavin and mirostrobin are best, and the inventor finds that when the proportion of water is high, nitrogen is difficult to blow, liquid is turbid, and the liquid is difficult to blow, so that result errors are large.
Example 4
The detection method of this example is substantially the same as that of example 1, except thatMeanwhile, the wet rice flour is used as a sample, and dSPE, MAS-Q, dSPEEMR-Lipid and dSPEEMR-Lipid + NaCl/MgSO are respectively adopted in the sample pretreatment 4 The results of recovery of toxoflavin and mirostrobin for the four different purification adsorbents are shown in table 4. Wherein dSPEEMR-Lipid + NaCl/MgSO 4 Is QuEChERS dSPE EMR-Lipid (Agilent technologies, guangzhou), polish Tube-NaCl/MgSO 4 (Agilent technologies, inc., guangzhou) the combination of the two adsorbents is carried out by treating with QuEChERS dSPE EMR-Lipid, and then with Polish Tube-NaCl/MgSO 4 Processing; each adsorbent referred to in this example was used in a predetermined amount of commercial adsorbent.
The results show that when dSPE and MAS-Q are used as purifiers, the recovery rate of target compounds is lower than 30%, the main components of dSPE and MAS-Q are PSA (N-propyl ethylene diamine) and C18 (octadecyl bonded silica gel), because the PSA adsorbent can remove organic acid, pigment and saccharide impurities in a sample matrix, the C18 adsorbent can remove nonpolar interferents such as fat and esters, and the PSA and C18 can remove the target compounds in the purification process, so that the recovery rates of toxoflavin and mircothric acid are reduced. And dSPEEMR-Lipid + NaCl/MgSO 4 When the microbial contamination purifying agent is used as a purifying agent, the recovery rates of toxoflavin and mircotiana acid can reach more than 80%, dSPE EMR-Lipid is independently adopted, the operation is simple, and the sample recovery rate is higher.
TABLE 4 Effect of different detergent combinations on recovery of toxoflavin and mircotoxicillin acid
Example 5
The detection method of this example is substantially the same as that of example 1, except that wet rice flour is used as a sample, and the number of extractions is 1, 2, and 3, respectively, in the sample pretreatment. The results of recovery of toxoflavin and mirostrobin are shown in FIG. 3. Experiments show that the recovery rate of the sample is optimal after two times of extraction.
Example 6
The maximum absorption wavelengths of the diode array detector for the mirinomycesic acid and the toxoflavin are respectively 258nm, 267nm and 300nm when the diode array detector is used for analyzing.
This example is the same as example 1 except that wet rice flour is used as the sample, 258nm, 267nm and 300nm are used as the detection wavelength in the chromatographic analysis, and the spectrogram is shown in FIG. 4-1 and FIG. 4-2. The results show that the two components of the zymotic acid and the toxoflavin at 258nm have larger absorption and the chromatographic separation degree is more than 1.5, so that the chromatographic analysis requirements can be well met.
Example 7
This example is substantially the same as example 1 except that wet rice flour is used as a sample, and during chromatography, formic acid, acetic acid and phosphoric acid are selected as mobile phase B to adjust pH to 3.0. The chromatogram is shown in FIG. 5. When formic acid is used as the acidity regulator, the response signal of the target compound is strong, the number of the mixed peaks is small, and the separation effect is good.
Example 8
The detection method of this example is substantially the same as that of example 1, except that wet rice flour is used as a sample, the pH of the mobile phase B is adjusted to 2.5, 3.0 and 3.5 respectively during chromatography, and the chromatogram is shown in fig. 6. It was found that the mobile phase B had a pH of both pH2.5 and pH3.0, the better the resolution of the target, while the lower the pH, the more damaging the column and the instrument and the narrower the range of column selection. Therefore, an aqueous solution adjusted to pH3.0 with formic acid is more preferable as the mobile phase B.
In conclusion, by adopting the detection method disclosed by the invention, on one hand, the problem of impurity interference in different food matrixes can be solved; on the other hand, by adopting the specific sample pretreatment process and chromatographic analysis conditions, the toxoflavin and the fermentation broth acid can be effectively separated, and the method has better sensitivity, precision and accuracy by verifying the methodological indexes such as a linear equation, a detection limit, a quantification limit, a recovery rate and the like, and provides an accurate, efficient, simple and convenient method for simultaneously detecting the contents of toxoflavin and fermentation broth acid in food.
It will be appreciated by those skilled in the art that modifications and adaptations to the invention may be made in light of the teachings of the present disclosure. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.
Claims (7)
1. A method for simultaneously detecting the content of flavonol and the content of fermentation broth acid in food is characterized by comprising the following steps:
1) Pretreating a sample
Extracting the sample twice, vortexing with 80% -90% methanol water solution for 2-5min, performing ultrasound for 10-15min, centrifuging, sucking the supernatant into a centrifuge tube pre-filled with dSPE EMR-Lipid adsorbent, vortexing for 2-5min, centrifuging, and taking the supernatant;
mixing the supernatants obtained by the two extractions, performing nitrogen blowing treatment on the obtained supernatant, performing constant volume with methanol, and filtering with a filter membrane to obtain a treated sample; the sample comprises a grain fermented product, a potato product, tremella and/or black fungus;
2) Carrying out chromatographic analysis on the treated sample obtained in the step 1), wherein the chromatographic conditions comprise: the chromatographic column is a C18 chromatographic column; the mobile phase comprises a mobile phase A and a mobile phase B, wherein the mobile phase A is methanol, and the mobile phase B is water with the pH value of 2.5-3.0; the detection wavelength is 258nm; the gradient elution procedure was:
0-5min, 20% of mobile phase A and 80% of mobile phase B;
5-6min, mobile phase A20% → 90%, mobile phase B80% → 10%;
6-14min, mobile phase A90%, mobile phase B10%;
14-15min, mobile phase A90% → 20%, mobile phase B10% → 80%;
15-20min, 20% of mobile phase A and 80% of mobile phase B;
the above percentages all refer to volume percentages in the mobile phase;
3) And (3) quantitatively analyzing the content of the flavonol and the mirinomycin acid in the sample according to a pre-drawn standard curve and the detection result obtained by the chromatographic analysis in the step 2).
2. The method for simultaneously detecting the content of flavochrome and the content of mirostrobin in the food according to claim 1, wherein in the step 2), the pH of the water serving as the mobile phase B is 3.0.
3. The method for simultaneously detecting the content of flavonol and the content of mirinomycesic acid in the food according to claim 1 or 2, wherein in the step 2), the pH of the water as the mobile phase B is adjusted to 3.0 by using formic acid.
4. The method for simultaneously detecting the content of flavochrome and the content of mirostrobin in the food according to claim 3, wherein in the step 1), the concentration of the methanol aqueous solution is 80%.
5. The method for simultaneously detecting the content of flavochrome and the content of mirostrobin in the food according to claim 1 or 2, wherein the amount of the methanol aqueous solution used in the step 1) is 10ml per 2g of the sample.
6. The method for simultaneously detecting the content of flavochrome and the content of mirostrobin in the food according to claim 1 or 2, wherein in the step 2), the chromatographic conditions further comprise: the flow rate is 1mL/min; the column temperature is 30 ℃; the amount of sample was 10. Mu.L.
7. The method for simultaneously detecting the content of flavonol and the content of mirinomycesic acid in the food according to claim 1, wherein the quantitative analysis is performed by an external standard method.
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