CN115656349A - Method for determining 55 biotoxins in nut food - Google Patents
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Abstract
The invention discloses a method for measuring 55 biotoxins in nut food, which comprises the following steps: (1) sample pretreatment; (2) QuEChERS purification: adding the supernatant solution into a centrifugal tube containing a QuEChERS purifying agent, uniformly mixing and centrifuging, taking the supernatant, adding a diluent, uniformly mixing, and filtering through an organic filter membrane to obtain a solution to be detected for later use; wherein, the raw material of the QuEChERS purifying agent comprises C 18 PSA and anhydrous sodium sulfate; (3) preparing a substrate labeling solution; (4) analyzing a sample; and (5) drawing a matrix marking curve. The method for determining 55 biotoxins in nut food improves the front part of a QuEChERS sampleThe method optimizes chromatographic and mass spectrum conditions, and establishes a method for simultaneously detecting 55 mycotoxins in nut foods. The method has the characteristics of simplicity, convenience, rapidness, accuracy, good reproducibility and high sensitivity, and can meet the requirements of high-throughput rapid screening confirmation and accurate quantification of mycotoxins in nut products.
Description
Technical Field
The invention relates to the technical field of food safety detection, in particular to a method for determining 55 biotoxins in nut food.
Background
Biotoxins, also known as natural toxins, are non-self-replicating toxic chemical substances secreted by living organisms and have toxic effects on other biological species. The growth and propagation of fungi may occur in the agricultural products during the cultivation and storage processes, so that various biotoxins are generated, and the mycotoxins are detected in various agricultural products such as wheat, corn, rice, tomatoes, peaches and the like. With the rapid development of Chinese economy, the consumption of nut food is continuously increased.
Nut food is easy to be polluted by fungi in the processes of production, processing, transportation, storage and the like, in recent years, the problem of exceeding the mycotoxin of the nut food is frequently found, and the safety problem of the nut food is more and more concerned by consumers and relevant departments. At present, the detection methods for mycotoxin in food mainly comprise an enzyme-linked immunosorbent assay, a high performance liquid chromatography, a gas chromatography-mass spectrometry and a liquid chromatography-mass spectrometry, but none of the methods can realize the accurate qualitative and quantitative determination of trace amount of mycotoxin in complex matrix of nut food. Therefore, the establishment of a high-throughput and non-targeted rapid detection method for nut food mycotoxin has important significance for guaranteeing food safety in China and health of people.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide a method for measuring 55 biotoxins in nut food, thereby overcoming the defects of low speed, low efficiency, low accuracy and the like in the detection of mycotoxins in the nut food.
To achieve the above object, the present invention provides a method for measuring 55 biotoxins in nut food, comprising the steps of:
(1) Sample pretreatment: accurately measuring a nut sample, adding ultrapure water into the sample, uniformly mixing, standing, adding acetic acid acetonitrile, mixing, adding sodium chloride, oscillating and centrifuging;
(2) QuEChERS purification: adding the supernatant solution into a centrifugal tube containing a QuEChERS purifying agent, uniformly mixing and centrifuging, taking the supernatant, adding a diluent, uniformly mixing, and filtering through an organic filter membrane to obtain a solution to be detected for later use; wherein, the raw material of the QuEChERS purifying agent comprises C 18 PSA and anhydrous sodium sulfate;
(3) Preparing a substrate labeling solution: preparing standard solutions for adding the standard with different concentrations, taking a blank matrix sample, adding the standard solution for adding the standard, uniformly mixing, standing for a period of time, and preparing the matrix standard solution for later use by adopting the extraction method in the step (1) and the purification method in the step (2);
(4) And (3) sample analysis: detecting the content of biotoxin in the solution to be detected obtained in the step (2) by adopting an ultra-high performance liquid chromatography-high resolution mass spectrometry combined method;
(5) Drawing a matrix standard curve: and (5) measuring the matrix labeling solutions with different concentrations prepared in the step (3) by adopting the detection conditions in the step (4) to obtain a matrix labeling curve, and simultaneously realizing qualitative and quantitative analysis by utilizing a matrix labeling method.
Preferably, in the technical scheme, 1-5g of nut sample is accurately weighed in the step (1) and added into a centrifuge tube, 1-10mL of ultrapure water is added, vortex mixing is carried out for 0.5-5min, standing is carried out for 10-60min, 1-5mL of 1% acetic acid acetonitrile is added, vortex mixing is carried out for 0.5-5min, 0.5-3g of sodium chloride is added, oscillation mixing is carried out, oscillation extraction is carried out on an oscillator for 15-60min, and centrifugation is carried out for 5-20min at 1-10 ℃ and 1000-20000 rpm.
Preferably, in the above technical scheme, in the step (2), 1-5mL of the upper layer solution is transferred into a centrifuge tube containing a QuEChERS purifying agent, the mixture is subjected to vortex mixing for 0.5-5min, the mixture is subjected to centrifugation at 1000-10000rpm for 1-10min, the mixture is taken out and subjected to vortex mixing for 0.5-5min, the mixture is subjected to centrifugation at 1000-10000rpm for 1-10min, 0.5-2.5mL of the upper layer solution is transferred into the centrifuge tube, 0.5-2.5mL of diluent is added, the mixture is subjected to vortex mixing for 10-60s, all the solution is absorbed by an injector, and the solution is filtered by an organic phase filter membrane to obtain the solution to be detected.
Preferably, in the above technical solution, the queechers purifying agent raw material C 18 PSA and anhydrous sodium sulfate in a mixing mass ratio of 1-3.
Preferably, in the above technical scheme, the QuEChERS purifying agent raw material C 18 PSA and anhydrous sodium sulfate in a mass ratio of 2.
Preferably, in the above technical solution, the dilution solution in step (2) contains at least 5mmoL ammonium formate and 0.1% aqueous methanol solution with a formic acid volume ratio of 5.
Preferably, in the above technical scheme, the step (3) is kept standing for 20-60min.
Preferably, in the above technical solution, the liquid chromatography conditions in step (4) are as follows: a Thermo Accucore RP-MS liquid chromatography column; a mobile phase A: 5mmoL ammonium formate and 0.1% formic acid in methanol in water; and (3) mobile phase B: an aqueous methanol solution containing 5 mmols of ammonium formate and 0.1% formic acid; flow rate: 0.30mL/min; column temperature: 30.0 ℃; sample introduction amount: 5 mu L of the solution; gradient elution mode is adopted.
Preferably, in the above technical solution, the elution procedure of the gradient elution is as follows: 0min:5% solution A,95% solution B;12min:95% of solution A and 5% of solution B;15min;95% of solution A and 5% of solution B;18min:5% solution A,95% solution B.
Preferably, in the above technical solution, the conditions of the liquid mass spectrum in step (4) are as follows: an ion source: heating an electrospray ion source; ion source temperature: 350 ℃; flow rate of sheath gas: 40a.u.; flow rate of auxiliary gas: 10a.u.; spraying voltage: 3.5kV; capillary temperature: 320 ℃; scanning mode: full MS and dd-MS2; full MS mode: the resolution is 70000; the scanning range is 100-900 m/z; AGC target is 1e6 a.u; the maximum injection time is 200ms; dd-MS2 mode: resolution is 17500; AGC target 5e5 a.u; the maximum injection time was 60ms; topN is 1a.u.; the isolation window is 2.0m/z; the gradient normalized collision energies were 20eV, 40eV, and 60eV.
Compared with the prior art, the invention has the following beneficial effects: the method for determining 55 biotoxins in nut food improves the pretreatment method of QuEChERS samples, optimizes chromatographic and mass spectrum conditions, and establishes a method for simultaneously detecting 55 mycotoxins in nut food. The method has the characteristics of simplicity, convenience, rapidness, accuracy, good reproducibility and high sensitivity, and can meet the requirements of high-throughput rapid screening confirmation and accurate quantification of mycotoxins in nut products.
Drawings
FIG. 1 is a Zea mays alcohol isomer α/β chromatogram according to the present invention;
FIG. 2 is a zearalenol isomer α/β chromatogram according to the present invention.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations such as "comprises" or "comprising", etc., will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
The reagents and instrumentation used in the following examples are as follows:
1. primary reagent
Analytically pure sodium chloride and anhydrous sodium sulfate, purchased from Guangdong Guanghua science and technology GmbH; chromatographic grade methanol, acetonitrile, acetic acid, available from TEDIA tiandi, usa; analytically pure ammonium formate, purchased from national chemical group, chemical reagents, ltd; chromatographically pure formic acidOctadecyl bonded silica gel adsorbent (C) 18 40-63 μm), N-propylethylenediamine (primary secondary amine, PSA, 40-63 μm), available from CNW, germany. A mixed standard solution of 77 mycotoxins in acetonitrile is purchased from detection Limited of petrochemical research institute of Guangxi province, and the information of 55 mycotoxins standard products listed as detection targets of the research is shown in Table 1.
TABLE 1 Standard information on 55 mycotoxins
2. Main instrument
Thermo UltiMate 3000 ultra high performance liquid chromatography tandem Q-active quadrupole/electrostatic field orbitrap high resolution mass spectrometer, thermo Accucore RP-MS liquid chromatography column (2.1 mm x 100 mm,2.6 μm) available from Thermo Fisher Scientific, usa; oasis PRiME HLB (3cc, 150mg) solid phase extraction column, available from waters corporation, usa; vortex mixer model Vortex-Genie2 from Scientific Industries, USA; milli-Q Integral 10 ultra pure water machine, available from Millipore corporation, USA; SA300 multifunction shaker available from Yamato corporation of japan; SIGMA 3-18KS desk-top high speed refrigerated centrifuge available from SIGMA corporation, germany; an L420 desk-top low-speed centrifuge, available from Hunan instruments laboratory development Co., ltd; ML203T electronic balance, available from Mettler-Toledo, switzerland; 0.22 μm hydrophobic PTFE needle filter, available from Shanghai' an spectral laboratory technologies.
3. Chromatographic conditions
A chromatographic column: a Thermo Accucore RP-MS liquid chromatography column; mobile phase A: a solution of 5mmoL ammonium formate and 0.1% formic acid in methanol in water (95,v; mobile phase B: a solution of 5mmoL ammonium formate and 0.1% formic acid in methanol in water (5, 95,v; flow rate: 0.30mL/min; column temperature: 30.0 ℃; sample introduction amount: 5 mu L of the solution; the gradient elution procedure is shown in table 2.
TABLE 2 gradient elution procedure
The bonded phase of the Thermo Accucore RP-MS chromatographic column adopted in the research is a carbon chain with optimized length, and the surface of silica gel can be effectively covered, so that the non-hydrophobic interaction is reduced, a better column effect is obtained, and the tailing is reduced. At the same time, the isomers alpha-Zearalenol (alpha-Zearalanol), alpha-Zearalenol (alpha-Zearalenol), beta-Zearalanol (beta-Zearalanol) and beta-Zearalenol (beta-Zearalenol) can be completely separated from each other at baseline, as shown in fig. 1 and fig. 2.
Under the chromatographic conditions, the 55 mycotoxins can be well separated within 18 minutes, the retention of each mycotoxin to be detected is good, the peak shapes are smooth and symmetrical, and the retention time of the 55 mycotoxins is shown in table 3.
Table 3 mass spectral data of 55 mycotoxins
4. Conditions of Mass Spectrometry
An ion source: heating an electrospray ionization source (HESI); ion source temperature: 350 ℃; flow rate of sheath gas: 40a.u.; flow rate of auxiliary gas: 10a.u.; spraying voltage: 3.5kV; capillary temperature: at 320 ℃. Scanning mode: full MS and dd-MS2.Full MS mode: the resolution is 70000; the scanning range is 100-900 m/z; AGC target is 1e6 a.u; maximum Injection Time (IT) 200ms; dd-MS2 mode: resolution is 17500; AGC target 5e5 a.u; maximum Injection Time (IT) 60ms; topN is 1a.u.; the isolation window is 2.0m/z; gradient Normalized Collision Energy (NCE) was 20eV, 40eV, and 60eV.
In the research, first-stage mass spectrum Full scanning is adopted, mass spectrum detection is carried out on 55 mycotoxin standard substances in a Full-MS mode, and actual measurement accurate molecular weights of 55 mycotoxin parent ions can be obtained. When the parent ion intensity reaches the set threshold (1X 10) 6 ) And the error between the measured mass and the theoretical mass is +/-5 multiplied by 10 -6 Within range, the instrument will enter a secondary mass spectrometry scan (dd-MS 2 mode) to obtain secondary mass spectra of 55 mycotoxins. In the research, fragment ions (shown in table 3) with higher actual measurement mass and response of parent ions and fragment ions at the first 3 positions are selected and combined with the retention time of liquid chromatography to carry out qualitative and quantitative analysis on target compounds. According to the research, the Q-active high-resolution mass spectrometer is used for setting the gradient normalized collision energy, so that the reproducibility of each experiment can be ensured, and the setting of a mass spectrometry method and the optimization process of the collision energy are simplified. The finally obtained mass spectrum data of 55 mycotoxins such as acquisition modes, ionization modes, theoretical mass, actually measured mass, daughter ions, retention time and the like are shown in a table 3. The results show that the error range between the measured mass number and the theoretical mass number of the 55 mycotoxins is-1.4X 10 -6 ～1.0×10 -6 Are all within +/-5 multiplied by 10 -6 Meets the qualitative and quantitative requirements of high-resolution mass spectrum within the range.
5. Sample pretreatment
(1) Sample extraction: accurately weighing 2.00g of nut sample into a 15mL centrifuge tube, adding 2mL of ultrapure water, uniformly mixing for 1min by vortex, and standing for 30min. Adding 2mL of 1% (v: v) acetonitrile acetate, vortex mixing for 1min, adding 1g of sodium chloride, immediately covering and shaking for mixing, and shaking and extracting on a shaker for 30min. Centrifugation was carried out at 10000rpm for 10min at 4 ℃.
(2) QuEChERS purification: 1mL of the supernatant was transferred to a column containing QuEChERS scavenger (0.2 g C) 18 0.1g of PSA, 0.5g of anhydrous Na 2 SO 4 ) The mixture was vortexed for 1min, centrifuged at 4000rpm for 5min, taken out, vortexed again for 1min, centrifuged at 4000rpm for 5min, 0.5mL of supernatant was transferred to a 15mL centrifuge tube, 0.5mL of a diluent (5And (4) analyzing by using a high-resolution mass spectrum system.
The improved sample treatment method has the following advantages: (1) 1% acetonitrile acetate is used as a buffer solution, so that the operation is simpler and the extraction efficiency is higher. (2) Sodium chloride is used for salting out and layering, so that the influence of heat release of anhydrous magnesium sulfate in water on mycotoxin is avoided, and the recovery rate of the method is improved. (3) Selection C 18 PSA and anhydrous sodium sulfate are used as purification fillers, polar interference substances such as saccharides and organic acids and non-polar interference substances such as lipids, sterols and pigments in the nut food can be effectively removed, so that the matrix effect of the interference substances on mycotoxin is reduced, and higher accuracy and precision are obtained; the GCB filler is not selected, so that the recovery rate is greatly reduced due to the fact that GCB adsorbs mycotoxin with a planar structure, and the method is suitable for detection and analysis of more mycotoxins with different structural properties. (4) Optimizes the whole pretreatment process, accelerates the analysis speed, and optimally controls the optimal dosage and proportion (0.2 g C) of each filler 18 0.1g of PSA and 0.5g of anhydrous sodium sulfate), the reagent dosage is greatly reduced, and the detection cost is saved.
6. Method and limit of quantitation
The method is characterized in that a matrix standard adding method is adopted for quantification, namely, a matched blank matrix sample is selected, standard substances with different concentrations are added, the blank matrix sample and a detection sample are extracted and purified together according to a pretreatment method, and then sample introduction is carried out, and a linear equation is fitted by taking the addition concentration as an X axis and the peak area as a y axis and is used for result quantification of a sample to be detected. The quantitative method has low cost, does not need to purchase expensive isotope internal standards, and has high recovery rate, and the accuracy of the quantitative result is higher than that of the matrix matching curve quantitative method. In the study, peanuts and macadamia nuts are selected as blank matrixes to prepare a standard addition curve, and the result is shown in table 4, wherein 55 mycotoxins are in the standard addition range of 0.10-80.0 mu g/kg, the linear correlation coefficient is good, and R is 2 Are all more than or equal to 0.990, and meet the requirement of accurate method quantification.
TABLE 4 Linear concentration, correlation coefficient and equation for 55 mycotoxin substrate calibration curves
Because the baseline noise of the high-resolution mass spectrometry detection system is usually very low, the signal-to-noise ratio of most mycotoxins is very high when standard substances are used for sample injection, the sensitivity is very high, and the quantitative limit determined according to the signal-to-noise ratio of the standard substances being more than or equal to 10 is too low to be achieved in actual sample detection. Therefore, the research determines the quantitative limit by a method of adding standard substances into the matrix extracting solution, and determines the lowest standard adding concentration of each mycotoxin which meets the signal-to-noise ratio of more than or equal to 10 and the recovery rate of 70-120% as the quantitative limit of the method. The quantitative limit of the method for the 55 mycotoxins in the research is 0.10-40.0 mu g/kg.
7. Recovery and precision
In the research, 2 nut samples of peanuts and macadamia nuts are selected for method verification, and the standard recovery rate and the precision of 55 mycotoxins in the two samples are mainly investigated. Adding standard substances according to 3 concentration levels of the quantitative limit, the 2.5-time quantitative limit and the 5-time quantitative limit, setting 3 parallel adding levels, processing according to a sample pretreatment method, detecting by using HPLC-HRMS, and quantifying by using a matrix standard adding method. The results are shown in table 5, the standardized recovery rate of 55 mycotoxins in different substrates and different concentration levels is 70.3-120.0%, and the relative standard deviation is 0.3-19.5% (n = 3), which indicates that the 55 mycotoxins have better recovery rate and precision under different substrates and different added concentration conditions, and meet the requirements of the food physicochemical detection standard for laboratory quality control.
TABLE 5 limit of quantitation, recovery and precision of 55 mycotoxins in peanuts and Hawaii fruits
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A method for determining 55 biotoxins in nut based food products, comprising the steps of:
(1) Sample pretreatment: accurately weighing a nut sample, adding ultrapure water into the sample, uniformly mixing, standing, adding acetic acid acetonitrile, mixing, adding sodium chloride, oscillating and centrifuging;
(2) QuEChERS purification: adding the supernatant solution into a centrifugal tube containing a QuEChERS purifying agent, uniformly mixing and centrifuging, taking the supernatant, adding a diluent, uniformly mixing, and filtering through an organic filter membrane to obtain a solution to be detected for later use; wherein, the raw material of the QuEChERS purifying agent comprises C 18 PSA and anhydrous sodium sulfate;
(3) Preparing a substrate labeling solution: preparing standard solutions for adding the standard with different concentrations, taking a blank matrix sample, adding the standard solution for adding the standard, uniformly mixing, standing, and preparing the matrix standard solution for later use by adopting the extraction method in the step (1) and the purification method in the step (2);
(4) And (3) sample analysis: detecting the content of biotoxin in the solution to be detected obtained in the step (2) by adopting an ultra-high performance liquid chromatography-high resolution mass spectrometry combined method;
(5) Drawing a matrix standard curve: and (4) measuring the substrate labeling solutions with different concentrations prepared in the step (3) by adopting the detection conditions in the step (4) to obtain a substrate labeling curve, and simultaneously realizing qualitative and quantitative analysis by using a substrate labeling method.
2. The method for determining 55 biotoxins in nut food according to claim 1, wherein in step (1), 1-5g of nut sample is accurately weighed into a centrifuge tube, 1-10mL of ultrapure water is added, the mixture is vortexed and mixed for 0.5-5min, the mixture is kept still for 10-60min, 1-5mL of 1% acetonitrile acetate is added, the mixture is vortexed and mixed for 0.5-5min, 0.5-3g of sodium chloride is added, the mixture is vortexed and mixed, the mixture is vortexed and extracted on a shaker for 15-60min, and the mixture is centrifuged at 1000-20000rpm and 1-10 ℃ for 5-20min.
3. The method for measuring 55 biotoxins in nut food as claimed in claim 1, wherein in the step (2), 1-5mL of the supernatant solution is transferred to a centrifuge tube containing a QuEChERS purifying agent, the mixture is subjected to vortex mixing for 0.5-5min, the mixture is subjected to centrifugation at 1000-10000rpm for 1-10min, the mixture is taken out and subjected to vortex mixing for 0.5-5min, the mixture is subjected to centrifugation at 1000-10000rpm for 1-10min, 0.5-2.5mL of the supernatant solution is transferred to the centrifuge tube, 0.5-2.5mL of a diluent solution is added, the mixture is subjected to vortex mixing for 10-60s, all the solution is sucked by a syringe, and the solution is filtered through an organic phase filter membrane to obtain the solution to be measured.
4. The method of claim 1 wherein said QuEChERS cleanser feedstock C is comprised of QuEChERS cleanser feedstock C 18 PSA and anhydrous sodium sulfate in a mixing mass ratio of 1-3.
5. The method for determining 55 biotoxins in nut food products according to claim 1 or 4, wherein said QuEChERS scavenger raw material C 18 PSA and anhydrous sodium sulfate in a mass ratio of 2.
6. The method of claim 1, wherein the dilution of step (2) comprises at least a 5 mmoL/v ratio of 5% aqueous methanol solution of 5mmoL ammonium formate and 0.1% formic acid.
7. The method of claim 1, wherein step (3) is performed for a period of 20-60min.
8. The method for determining 55 biotoxins in nut food products according to claim 1, wherein the liquid chromatography conditions in step (4) are: a Thermo Accucore RP-MS liquid chromatography column; mobile phase A: an aqueous methanol solution containing 5 mmols of ammonium formate and 0.1% formic acid; and (3) mobile phase B: 5mmoL ammonium formate and 0.1% formic acid in methanol in water; flow rate: 0.30mL/min; column temperature: 30.0 ℃; sample introduction amount: 5 mu L of the solution; gradient elution mode is adopted.
9. The method of claim 7 wherein the gradient elution is performed as follows: 0min:5% solution A,95% solution B;12min:95% of solution A and 5% of solution B;15min;95% of solution A and 5% of solution B; and (4) 18min:5% solution A,95% solution B.
10. The method of claim 1, wherein the conditions of the liquid mass spectrometry in step (4) are: an ion source: heating an electrospray ion source; ion source temperature: 350 ℃; flow rate of sheath gas: 40a.u.; flow rate of auxiliary gas: 10a.u.; spray voltage: 3.5kV; capillary temperature: 320 ℃; scanning mode: full MS and dd-MS2; full MS mode: the resolution is 70000; the scanning range is 100-900 m/z; AGC target is 1e6 a.u; the maximum injection time is 200ms; dd-MS2 mode: resolution is 17500; AGC target is 5e5 a.u; the maximum injection time was 60ms; topN is 1a.u.; the isolation window is 2.0m/z; the gradient normalized collision energies were 20eV, 40eV, and 60eV.
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