CN112946153B - Method for simultaneously determining multiple pollutants in plastic barreled vegetable oil - Google Patents
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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
- G01N2030/8872—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 impurities
Abstract
The invention discloses a method for simultaneously measuring various pollutants in plastic barreled vegetable oil, which comprises the following steps: (1) Extracting and purifying the edible oil sample by using an anion exchange adsorbent PAX as an adsorbing material through a dispersive micro solid phase extraction technology; (2) Separating the purified extract by C18 chromatographic column and methanol-0.05% ammonia water solution via gradient elution with concentration and flow rate, ionizing in positive and negative switching mode of electrospray ion source, and measuring in MS/MS multiple reaction monitoring mode (MRM); and (3) quantifying by an internal standard method. The method is suitable for simultaneous determination of 7 common 3 major (mycotoxins, bisphenols and alkylphenols) pollutants in the plastic barreled vegetable oil, makes up for the defect of single detection target object, and has the advantages of low detection limit and high detection accuracy.
Description
Technical Field
The invention relates to the technical field of food quality safety detection, in particular to a method for simultaneously determining various pollutants in plastic barreled vegetable oil.
Background
Aflatoxins are metabolites produced by the fungi aspergillus parasiticus and aspergillus flavus, and are one of mycotoxins. Aflatoxins are susceptible to contamination of a wide variety of crops and foods, and are often found in a variety of mildewed nuts, particularly peanuts, and their products. Aflatoxin was classified as a class i carcinogen by the cancer research institute of the world health organization in 1993. Aflatoxin B1 is one of the most toxic and carcinogenic substances. The countries around the world set allowable limit values for the content of aflatoxins, especially aflatoxin B1, in major food products. China also clearly defines the limit of mycotoxin in food, wherein the allowable limit value of aflatoxin B1 in peanuts and products thereof is defined to be 20 mu g/kg. Therefore, reliable and sensitive detection methods are needed to ensure food safety.
Bisphenol compounds are important raw materials for producing various polymer materials such as polycarbonate and the like, and are widely applied to industrial production such as food packaging materials and the like. Alkylphenols such as 4-nonylphenol and octylphenol are also widely used in the production of plastics to improve the properties of plastics. The two major compounds have the similar action with estrogen, can disturb the endocrine of human body, influence the reproductive and developmental functions, have toxic effects of teratogenesis, carcinogenesis, mutagenesis and the like, are easy to enrich and not easy to degrade, and have potential harm to human health and ecological environment. The European Union and China have strict regulations on the use and the limited quantity of bisphenol A, bisphenol S, bisphenol F and the like, for example, in plastic products in contact with food, the migration quantities of bisphenol A and bisphenol S are respectively less than 0.6mg/kg and 0.05mg/kg. In the processing and production of edible vegetable oil such as peanut oil, plastic products are used inevitably, and if the plastic products contain pollutants such as nonyl phenol, bisphenol A and the like, the plastic products may migrate and cause pollution in the process of contacting with the vegetable oil. The pollution conditions of the two pollutants in the plastic barreled vegetable oil at home and abroad are still in a risk monitoring stage, aiming at further proposing limit values to require the accumulation of basic data. Therefore, it is also desirable to establish reliable and sensitive detection methods.
At present, the research on the detection method of aflatoxin in vegetable oil is mature at home and abroad, the research on the detection method of bisphenol compounds and alkylphenol compounds is scattered, but different pretreatment methods and different instrument detection conditions are adopted for detection respectively, and the detection efficiency is limited. In view of the advantages of high selectivity, high sensitivity and the like of liquid chromatography-tandem mass spectrometry, detection research on trace pollutants in food generally takes a liquid chromatography-tandem mass spectrometry detection method as a mainstream. The pretreatment method may be liquid-liquid extraction, solid-phase extraction purification, GPC purification, or the like. However, it has been a difficult point of detection and research to extract and purify compounds with good lipid solubility from high-oil food.
The reported detection researches of the pollutants in the edible oil are all the detection of single-class compounds, and the simultaneous detection researches of mycotoxin, bisphenol and alkylphenol 3 large-class pollutants are not seen, so that the high-throughput detection of the multiple-class pollutants in the edible oil is of great significance.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention aims to provide the method for simultaneously detecting 3 types (mycotoxins, bisphenols and alkylphenols) of pollutants in the plastic barreled vegetable oil, the method for detecting the pollutants can be used for quickly and accurately simultaneously detecting and monitoring various pollutants in the edible oil by utilizing PAX adsorption, dispersion, micro-solid phase extraction and ultra-high performance liquid chromatography-tandem triple quadrupole mass spectrometry technology, has high recovery rate and good reproducibility, and can meet the trace analysis requirement.
The purpose of the invention is realized by the following technical scheme:
a method for simultaneously measuring multiple pollutants in plastic barreled vegetable oil comprises the following steps:
(1) Sample extraction and purification
Extracting and purifying the edible oil sample by using an anion exchange adsorbent PAX as an adsorbing material through a dispersive micro solid phase extraction technology;
(2) Liquid chromatography tandem triple quadrupole mass spectrometry
Performing elution separation on the extracting solution purified in the step (1) by adopting a C18 chromatographic column and a methanol-0.05% ammonia water solution through concentration gradient and flow velocity gradient, ionizing in an electrospray ion source positive and negative switching mode, and measuring in an MS/MS multiple reaction monitoring mode (MRM);
(3) Quantification by internal standard method
Preparing a series of mixed standard working solutions with concentration by using a methanol-water-formic acid mixed solution according to a gradient, wherein internal standard substances are added, and the internal standard substances are U-, [ 2 ] 13 C 17 ]Aflatoxin B1, bisphenol A-d 4 4-nonylphenol-d 4 ；
Under the same chromatographic mass spectrometry condition, equal-volume accurate sample injection is carried out, standard substances with different concentrations are collected to extract an ion chromatogram, each substance to be measured takes the ratio of the quantitative ion peak area to the corresponding internal standard substance quantitative ion peak area as a vertical coordinate, the ratio of the component concentration to the internal standard substance concentration as a horizontal coordinate, a standard working curve is drawn, and then the concentration of the substance to be measured in the sample is calculated through the standard curve.
Preferably, the liquid chromatography conditions of step (2):
mobile phase concentration and flow rate gradient elution procedures were as follows:
TABLE 1
Mobile phase: a is methanol and B is 0.05% (v/v) aqueous ammonia solution.
A chromatographic column: waters ACQUITY UPLC BEH C18 column, 50 mm. Times.2.1mm, 1.7 μm; or a Phenomenex kinetex C18 column, 100 mm. Times.3.0 mm,2.6 μm;
column temperature: 30-35 ℃, sample injection amount: 5 μ L.
Preferably, the tandem triple quadrupole mass spectrometry conditions of step (2): ionizing in an ESI positive ion mode at 0-1.5 min; ionizing in negative ion mode of 1.5-6min and ESI; multiple Reaction Monitoring (MRM) mode detection; the capillary voltage is 1.0kV; the ion source temperature is 150 ℃; the temperature of the solvent gas is 400 ℃; removing solvent gas: nitrogen gas, 800L/h; taper hole gas: nitrogen gas, 50L/h; collision gas: high-purity argon gas, 0.15mL/min; 2 secondary mass spectrum characteristic fragment ions with higher abundance are selected as qualitative and quantitative ions for each compound, and an internal standard substance is used for correction and quantification.
Preferably, the mass spectrometric conditions, the qualitative and quantitative ions of said contaminants and the corresponding internal standards are as follows:
TABLE 2
Preferably, the volume ratio of methanol, water and formic acid in the mixed solution in the step (3) is (48.0-49.9): (48.0 to 49.9): (0.2-1.0).
Preferably, the standard working solution is prepared according to the series of concentration mixing in the gradient in the step (3), wherein the concentration of aflatoxin B1 is 0.1, 0.2, 1.0, 5.0, 10.0 and 50.0 μ g/L, the concentration of bisphenol A, bisphenol B, bisphenol F, bisphenol S, 4-nonylphenol and octylphenol is 0.5, 1.0, 5.0, 20.0, 50.0 and 100 μ g/L, and the internal standard substance is added to make the concentration of the internal standard substance be 10 μ g/L.
Preferably, the sample extraction and purification of step (1): adding isotope internal standard into vegetable oil sample, dispersing with n-hexane, extracting with ammoniated methanol aqueous solution, dispersing and adsorbing with anion exchange adsorbent PAX, and eluting with acidified methanol to obtain extractive solution.
More preferably, the sample extraction and purification of step (1): taking a food oil sample, adding n-hexane and a micro-volume isotope internal standard mixed solution to enable the final concentration of an internal standard substance to be 5-20 mug/L, performing vortex dispersion, then adding a methanol-water-ammonia mixed solution, performing vortex extraction for 1-3min, performing centrifugation for 3-5min at 2500-5000r/min, transferring the lower layer of extract into a centrifuge tube containing 40-60mg of PAX (platelet activating X) which is activated in advance, performing vortex adsorption for 40-60s, performing centrifugation for 2-5min at 10000-12000r/min, discarding supernatant, adding the methanol-water-ammonia mixed solution, performing centrifugation for 2-5min at 10000-12000r/min, and discarding supernatant; then eluting with formic acid-methanol solution, centrifuging at 10000-12000r/min for 2-5min with vortex 40-60s, mixing the supernatants, placing in 30-40 deg.C water bath, slowly blowing nitrogen to concentrate to dryness, adding methanol-water solution, vortex for redissolving, and filtering with 0.22 μm polytetrafluoroethylene true pore filter membrane to obtain extractive solution.
Preferably, in the sample extraction and purification in the step (1), the volume ratio of the first added methanol-water-ammonia mixed solution is 60; the volume ratio of the methanol-water-ammonia water mixed solution added for the second time is (80); the volume ratio of the formic acid methanol solution is 2.
Preparing a standard solution: respectively weighing appropriate amount of standard substance and isotope standard substance (standard substance: aflatoxin B1, bisphenol A, bisphenol B, bisphenol S, bisphenol F, 4-nonylphenol, octylphenol; and internal standard substance: U-, [ solution ] 13 C 17 ]Aflatoxin B1, bisphenol A-d 4 4-nonylphenol-d 4 ) Preparing single standard stock solution with the mass concentration of 100mg/L by using methanol, and storing at the temperature of minus 20 ℃. Before use, the single standard stock solution is diluted into a mixed standard solution and a mixed isotope internal standard solution with required concentration by using methanol. A series of concentration mixed standard working solutions containing a concentration of an internal standard solution were prepared using a methanol-water-formic acid (49.8, v/v/v) mixed solution.
The method adopts PAX adsorption dispersion micro solid-phase extraction combined with the ultra-high performance liquid chromatography tandem triple quadrupole mass spectrometry to simultaneously detect 7 pollutants in the edible oil, and has the following beneficial effects compared with the prior art:
(1) Aiming at a sample matrix of edible oil, the invention uses anion exchange adsorbent (PAX) as an adsorbing material for the first time, and can quickly and efficiently extract aflatoxin B1, bisphenol A, bisphenol B, bisphenol S, bisphenol F, 4-nonylphenol and octylphenol in a sample by a dispersive micro solid-phase extraction technology, the method is simple and reliable, the recovery rate of the extracted target is high, and the trace analysis requirement can be met.
(2) Aiming at the defects that mycotoxin, bisphenol and alkylphenol pollutants in food are detected in a non-unified mode, and the detection methods are not unified, the invention firstly treats the three pollutants in a unified mode, establishes a detection method capable of simultaneously detecting 7 pollutants in 3 classes in edible oil, makes up the defect of single detection target object, and effectively improves the detection efficiency of the pollutants in the edible oil, and the method has the advantages of low detection limit, high detection accuracy and high quantitative limit of 0.2-1.0 mu g/kg for the 7 pollutants in the edible oil.
Drawings
FIG. 1 is an extracted ion chromatogram of aflatoxins B1 and 4-nonylphenol in a positive sample.
Detailed Description
The following examples are incorporated: the present invention will be described in further detail with reference to the simultaneous measurement of 7 kinds of contaminants such as aflatoxin B1 in peanut oil contained in plastic barrels, but the embodiment of the present invention is not limited thereto.
Example 1: simultaneous determination of 7 pollutants such as aflatoxin B1 in peanut oil in plastic barrels
(1) Sample extraction and purification conditions
Weighing 1.0g peanut oil sample, adding 3mL of n-hexane and a micro volume of isotope internal standard mixed solution (making the final concentration of the internal standard substance to be 10 μ g/L), performing vortex dispersion, then adding 1mL of methanol-water-ammonia water (60. Then, 2 times of elution are carried out with 2mL of methanoic acid (2, 98, v/v), 1mL each time, vortexed for 50s,12000r/min for 2min, the supernatants are combined, placed in a water bath at 35 ℃ and slowly concentrated to dryness by nitrogen blowing, 1.0mL of methanol-water (50, v/v) is added, vortexed for redissolution, and passed through a 0.22 μm Teflon true pore filter, and the filtrate is subjected to HPLC tandem mass spectrometry.
(2) Chromatographic separation and mass spectrum detection conditions
A chromatographic column: waters ACQUITY UPLC BEH C18 column (50 mm. Times.2.1mm, 1.7 μm).
Mobile phase: a is methanol and B is 0.05% (v/v) aqueous ammonia solution.
Column temperature: at 35 deg.c.
Sample introduction amount: 5 μ L.
Concentration and flow rate gradient elution procedures are shown in table 1.
Ionizing in an ESI positive ion mode at 0-1.5 min; ionizing in negative ion mode of 1.5-6min and ESI; multiple Reaction Monitoring (MRM) mode detection;
the capillary voltage is 1.0kV; the ion source temperature is 150 ℃; the temperature of the solvent gas is 400 ℃; removing solvent gas: nitrogen gas, 800L/h; taper hole gas: nitrogen gas, 50L/h; collision gas: high purity argon, 0.15mL/min.
2 secondary mass spectrum characteristic fragment ions with higher abundance are selected as qualitative and quantitative ions for each compound, and an internal standard substance is used for correction and quantification. The mass spectrometric conditions, qualitative and quantitative ions and the corresponding internal standards for the 7 contaminants are shown in table 2.
(3) Quantification by internal standard method
Preparing a series of standard substance solutions according to gradients, wherein the concentration of aflatoxin B1 is 0.1, 0.2, 1.0, 5.0, 10.0 and 50.0 mu g/L, the concentration of bisphenol A, bisphenol B, bisphenol F, bisphenol S, 4-nonylphenol and octylphenol is 0.5, 1.0, 5.0, 20.0, 50.0 and 100 mu g/L, a certain amount of internal standard substance is added to ensure that the concentration of the internal standard substance is 10 mu g/L, under the same chromatographic mass spectrum condition, equal-volume accurate sample injection is carried out, standard substance extraction ion chromatograms with different concentrations are collected, each substance to be detected uses the ratio of the peak area of the quantitative ion peak area to the peak area of the corresponding internal standard substance as a vertical coordinate, and the ratio of the component concentration to the internal standard substance as a horizontal coordinate, a standard working curve is drawn, and the concentration of the substance to be detected in the sample is calculated through the standard curve.
(4) Selectivity and certainty
Taking 15 negative peanut oil samples, detecting according to the sample pretreatment method and the instrument conditions of the invention, and inspecting whether the other components in the samples interfere with the determination of the object to be detected. The result shows that the coexisting substance in the sample solution does not interfere with the qualitative and quantitative determination of the substance to be detected because of the high selectivity of the triple quadrupole mass spectrometry.
(5) Linear relationship, detection limit and matrix effect
The linear regression equation, correlation coefficient, detection limit, quantitation limit, and matrix effect for the 7 analytes are shown in Table 3. Therefore, the linear relation of each target object to be detected in the corresponding concentration range is good, and the correlation coefficient is larger than 0.99. The detection limit is between 0.06 and 0.3 mu g/L, the quantification limit is between 0.2 and 1.0 mu g/kg, and the matrix effect is between 0.88 and 1.11.
TABLE 3 Linear relationship, detection limits and matrix Effect of peanut oil sample determination
(6) Method recovery, accuracy and precision
Method recovery, accuracy and precision were investigated by an additive recovery test of negative samples (n = 6). That is, 3 concentration levels of the mixed standard solution were added to each of the negative peanut oil samples, the samples were treated and measured under the conditions of the present invention, 6 tests were carried out, the intermediate addition concentration was measured continuously for 5 days, and the recovery rate, the day precision (n = 6) and the day precision (n = 5) were calculated, and the results are shown in table 4. It can be seen that at 3 standard concentrations, the recovery rate in the day is 81.1% -111.4%, and the precision in the day (n = 6) is between 3.1% -9.4%; the average recovery rate in the daytime is 87.4-106.5%, and the precision in the daytime (n = 5) is 7.3-13.0%. The method of the invention has the advantages of satisfactory recovery rate, good accuracy and precision.
TABLE 4 recovery and precision results of peanut oil sample determination
EXAMPLE 2 testing of a sample of real peanut oil
36 samples of commercially available plastic barreled peanut oil are measured by using the method of the embodiment 1, 27 samples detect the aflatoxin B1, the content of the aflatoxin B1 is between 0.6 and 78.2 mu g/kg, and 8 samples have the aflatoxin B1 content exceeding the limit value of national standard of 20 mu g/kg; 4-nonyl phenol was detected in 7 samples, with a content of 11.2-80.4. Mu.g/kg. The extracted ion chromatogram of the positive sample is shown in FIG. 1.
Claims (8)
1. A method for simultaneously measuring various pollutants in plastic barreled vegetable oil is characterized by comprising the following steps:
(1) Sample extraction and purification
Extracting and purifying the edible oil sample by using an anion exchange adsorbent PAX as an adsorbing material through a dispersive micro solid phase extraction technology; the sample extraction and purification: taking a vegetable oil sample, adding an isotope internal standard, dispersing by using normal hexane, extracting by using an ammoniated methanol aqueous solution, performing dispersion adsorption by using an anion exchange adsorbent PAX, and eluting by using acidified methanol to obtain an extracting solution;
(2) Liquid chromatography tandem triple quadrupole mass spectrometry
Performing elution separation on the extracting solution purified in the step (1) by adopting a C18 chromatographic column and a methanol-0.05% ammonia water solution through concentration gradient and flow velocity gradient, ionizing in an electrospray ion source positive and negative switching mode, and measuring in an MS/MS multi-reaction monitoring mode; the C18 chromatographic column is a Waters ACQUITY UPLC BEH C18 chromatographic column or a Phenomenex kinetex C18 chromatographic column;
(3) Quantification by internal standard method
Preparing a series of mixed standard working solutions with concentration by using a methanol-water-formic acid mixed solution according to a gradient, wherein internal standard substances are added, and the internal standard substances are U-, [ 2 ] 13 C 17 ]Aflatoxin B1, bisphenol A-d 4 4-nonylphenol-d 4 ；
Under the same chromatographic mass spectrum condition, carrying out equal-volume accurate sample injection, collecting standard substance extraction ion chromatograms with different concentrations, drawing a standard working curve by taking the ratio of the peak area of the quantitative ion to the peak area of the quantitative ion of the corresponding internal standard substance as a vertical coordinate and the ratio of the component concentration to the internal standard substance concentration as a horizontal coordinate, and further calculating the concentration of the substance to be detected in the sample through the standard curve;
the liquid chromatography conditions of step (2):
mobile phase concentration and flow rate gradient elution procedures were as follows:
mobile phase: a is methanol and B is 0.05% v/v aqueous ammonia solution;
the pollutants are aflatoxin B1, bisphenol A, bisphenol B, bisphenol F, bisphenol S, 4-nonylphenol and octylphenol.
2. The method of claim 1, wherein the liquid chromatography conditions are:
a chromatographic column: waters ACQUITY UPLC BEH C18 column, 50 mm. Times.2.1mm, 1.7 μm; or a Phenomenex kinetex C18 column, 100 mm. Times.3.0 mm,2.6 μm;
column temperature: 30-35 ℃, sample injection amount: 5 μ L.
3. The method of claim 1 or 2, wherein step (2) the tandem triple quadrupole mass spectrometry conditions: ionizing in an ESI positive ion mode at 0-1.5 min; ionizing in negative ion mode of 1.5-6min and ESI; the capillary voltage is 1.0kV; the ion source temperature is 150 ℃; the temperature of the solvent gas is 400 ℃; removing solvent gas: nitrogen gas, 800L/h; taper hole gas: nitrogen gas, 50L/h; collision gas: high-purity argon gas, 0.15mL/min; 2 secondary mass spectrum characteristic fragment ions with higher abundance are selected as qualitative and quantitative ions for each compound, and an internal standard substance is used for correction and quantification.
4. The method of claim 3, wherein the mass spectrometric conditions for the contaminants, the qualitative and quantitative ions and the corresponding internal standards are as follows:
5. the method according to claim 4, wherein the volume ratio of methanol, water and formic acid in the mixed solution in the step (3) is (48.0-49.9): (48.0 to 49.9): (0.2-1.0).
6. The method of claim 5, wherein the standard working solution is prepared in a gradient series of concentrations in step (3), wherein the concentration of aflatoxin B1 is 0.1, 0.2, 1.0, 5.0, 10.0, 50.0 μ g/L, and the concentration of bisphenol A, bisphenol B, bisphenol F, bisphenol S, 4-nonylphenol, and octylphenol is 0.5, 1.0, 5.0, 20.0, 50.0, 100 μ g/L, and an internal standard substance is added to make the concentration of the internal standard substance 10 μ g/L.
7. The method of claim 1 or 2, wherein the sample extraction and purification of step (1):
taking a food oil sample, adding normal hexane and a micro-volume isotope internal standard mixed solution to enable the final concentration of an internal standard substance to be 5-20 mu g/L, performing vortex dispersion, then adding a methanol-water-ammonia water mixed solution, performing vortex extraction for 1-3min, performing centrifugation for 3-5min at a speed of 2500-5000r/min, transferring the lower-layer extract to a centrifuge tube containing 40-60mg of PAX which is activated in advance, performing vortex adsorption for 40-60s, performing centrifugation for 2-5min at a speed of 10000-12000r/min, discarding supernatant, adding the methanol-water-ammonia water mixed solution, performing centrifugation for 2-5min at a speed of 10000-12000r/min, and discarding the supernatant; then eluting with formic acid-methanol solution, whirling 40-60s, centrifuging at 10000-12000r/min for 2-5min, mixing the supernatants, placing in 30-40 deg.C water bath, slowly blowing nitrogen to concentrate to dry, adding methanol-water solution, whirling for redissolving, and filtering with 0.22 μm polytetrafluoroethylene pinhole filter membrane to obtain extractive solution.
8. The method according to claim 7, wherein in the sample extraction and purification in step (1), the volume ratio of the first added methanol-water-ammonia mixed solution is 60; the volume ratio of the methanol-water-ammonia water mixed solution added for the second time is 80; the volume ratio of the formic acid methanol solution is 2.
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