CN107907600A - It is a kind of that the method for aflatoxin and flavouring agent in vegetable fat is measured based on liquid-liquid extraction Liquid Chromatography-Tandem Mass Spectrometry at the same time - Google Patents
It is a kind of that the method for aflatoxin and flavouring agent in vegetable fat is measured based on liquid-liquid extraction Liquid Chromatography-Tandem Mass Spectrometry at the same time Download PDFInfo
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- CN107907600A CN107907600A CN201711008538.7A CN201711008538A CN107907600A CN 107907600 A CN107907600 A CN 107907600A CN 201711008538 A CN201711008538 A CN 201711008538A CN 107907600 A CN107907600 A CN 107907600A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The method of aflatoxin and flavouring agent in vegetable fat is measured based on liquid-liquid extraction Liquid Chromatography-Tandem Mass Spectrometry at the same time the invention discloses a kind of, the method of the present invention can measure aflatoxin B1 in vegetable oil at the same time, aflatoxin B 2, aflatoxin G 1, aflatoxin G 2, Aflatoxins M1, aflatoxin M 2, vanillic aldehyde, methyl vanillin and Ethyl vanillin, sample is extracted through acetonitrile solvent, ultrasound assisted extraction, solution is extracted after n-hexane purifies, analyzed under gradient condition, target analytes compare carry out qualitative analysis under multiple-reaction monitoring pattern with retention time and ion pair information, quantified by external standard method.The advantages of this method：Required sample size and amount of reagent are few, and analyze speed is fast, high sensitivity, favorable reproducibility, can realize the detection of aflatoxin and common flavouring agent at the same time, and new detection method is provided to evaluate the quality safety of vegetable fat sample.
Description
Technical field
6 kinds of aflatoxin aflatoxin B1s (AFB1) in vegetable fat, Huang are measured at the same time the present invention relates to a kind of
Aspertoxin B2 (AFB2), aflatoxin G 1 (AFG1), aflatoxin G 2 (AFG2), Aflatoxins M1 (AFM1) and Huang
Aspertoxin M2 (AFM2)；The method of 3 kinds of flavouring agent vanillic aldehydes, methyl vanillin and Ethyl vanillin, belongs to and is supervised towards food
Survey technology field, and in particular to based on liquid-liquid extraction-liquid chromatography-tandem mass spectrometry positive ion mode assay method.
Background technology
Edible vegetable oil includes rapeseed oil, soybean oil, corn oil, peanut oil, olive oil, sesame oil, sunflower oil etc., is
The necessity of daily life, the mankind can take in a certain amount of vegetable oil in different forms daily, as the modern life is horizontal
Raising, requirement of the people not only to the quality of vegetable oil, nutrition, taste etc. be higher and higher, but also for vegetable oil
Edible safety also growing interest.Since crop seeds easily cause aflatoxin to produce in storing process, in view of yellow bent
The strong carcinogenicity of mould toxin, therefore whether there is aflatoxin residual to cause people more next in edible vegetable oil process
More concerns.In addition in grade, research shows in vegetable fat containing Pyrazine, furans, pyridines, pyroles, thiophene
The natural materials such as azole, phenols, ketone and aromatic compounds, very big, China GB2760-2011 is contributed to the fragrance of vegetable oil
《National food safety standard food additives use standard》Forbid adding any flavorant in clear stipulaties vegetable fat, be
The many businessmans in China are avoided in order to pursue the illegal addition spices of maximum benefit, so that there is " essence rice " and " essence steamed stuffed bun "
Etc. event, carrying out the detection of common flavouring agent for edible vegetable oil also gradually attracts people's attention.
At present, it is more to be related to the detection method of 6 kinds of aflatoxin of the invention and 3 kinds of flavouring agents, it is main to include efficiently
Liquid chromatography, gas chromatography, gas chromatography-mass spectrography, liquid chromatography-mass spectrometry, chromatography of ions etc., wherein liquid phase color
Concern of the spectrum-mass spectrography because being increasingly subject to people with high detection sensitivity.Carry out 6 kinds of yellow songs currently for plant oil matrix
Mould toxin AFB1, AFB2, AFG1, AFG2, AFM1, AFM2；3 kinds of flavouring agent vanillic aldehydes, methyl vanillin and Ethyl vanillin are same
When the method that detects in state, inside and outside do not appear in the newspapers still.
Edible vegetable oil is as one of most important diet, almost included in the three meals in a day of people.If vegetable oil
Middle aflatoxin content is exceeded or illegally adds flavouring agent, and long-term consumption will produce serious harm to health, therefore
Establish 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1, AFM2 in edible vegetable oil；3 kinds of flavouring agent vanillic aldehydes, first
Detection method has great importance while base vanillic aldehyde and Ethyl vanillin.
The content of the invention
The purpose of the present invention is based on above-mentioned prior art situation and provides a kind of quick, easy, efficiently, surveys at the same time
Determine 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1, AFM2 in vegetable fat；3 kinds of flavouring agent vanillic aldehydes, methyl are fragrant
The method of Lan Su and Ethyl vanillin.
Technical scheme：
One kind measures aflatoxin and fragrance in vegetable fat at the same time based on liquid-liquid extraction-liquid chromatography-tandem mass spectrometry
The method of agent, step are as follows：
(1) liquid-liquid extraction：Add Extraction solvent into grease to be measured and blank oil sample, the concussion that is vortexed, ultrasound and from
The heart, obtains supernatant liquor, to be clean；
(2) liquid liquid distribution purification：Purification flux is added in supernatant liquor, vortex oscillation, after centrifugation, takes subnatant,
Miillpore filter is crossed, obtains prepare liquid and bare substrate extracting solution；
(3) standard solution is prepared：First, by mass ratio be 1 vanillic aldehyde, methyl vanillin and Ethyl vanillin methanol
Dissolve and constant volume, obtain 1.0mg/mL standard reserving solutions, then with dilution in acetonitrile to 1.0mg/L hybrid standards storing solution 1；
Compound concentration is that aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2 standard of 0.1mg/L is molten respectively
Liquid, is hybrid standard storing solution 2；
Hybrid standard storing solution 1 and hybrid standard storing solution 2, mixing are drawn respectively；Diluted again with bare substrate extracting solution
To being respectively 10ng/mL, 20ng/mL, 40ng/mL, 80ng/mL, 160ng/mL containing vanillic aldehyde, AFB1 containing aflatoxin distinguishes
For the hybrid standard series of tasks solution of 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 2.0ng/mL, 5.0ng/mL；
(4) qualitative and quantitative analysis：The prepare liquid that step (2) is obtained enters liquid chromatography-tandem mass spectrometry instrument, and how anti-use is
Holotype monitoring, quantified by external standard method should be monitored；
A) qualitative analysis：Using LC-MS/MS methods measure sample and standard working curve is established, if detected in prepare liquid
The retention time of chromatographic peak is consistent with the retention time of respective standard material chromatographic peak, it is allowed to which deviation is less than 2.5%；Further
Compare the abundance for the qualitative ion of each component that concentration is close in sample to be tested and standard working solution, deviation is no more than as defined in table 1
Scope, then judge that there are corresponding sample to be tested in oil sample；
With respect to the maximum allowable offset of abundance of ions during 1 qualitative confirmation of table
| Relative ion abundance | ＞ 50% | 20%-50% | 10%-20% | ≤ 10% |
| The maximum deviation of permission | 20% | 25% | 30% | 50% |
B) quantitative analysis：Hybrid standard series of tasks solution is measured using LC-MS/MS methods, obtains corresponding standard solution
Chromatographic peak area, using the concentration of hybrid standard working solution as abscissa, using the peak area of chromatographic peak as ordinate, draw standard
Curve；Sample to be tested is measured with the same terms again, the chromatographic peak area of sample to be tested is obtained, is treated according to standard working curve
Survey the concentration of each component in liquid；Linear response range of the response of each component to be measured in standard working curve in sample to be tested
It is interior, if content goes beyond the scope, take sample to be tested to analyze again, then with dilution in acetonitrile to debita spissitudo post analysis；
(5) result calculates：
Calculation formula：
In formula (1)：
The content of component to be measured in X-oil sample, unit are μ g/kg；
The concentration of each component to be measured in the sample to be tested for c-read from standard working curve, unit is μ g/L；
The quality that m-oil sample weighs, unit g；
V-oil sample solution constant volume, unit mL.
The Liquid Chromatography-Tandem Mass Spectrometry test condition is as follows：
The chromatographic condition of the LC-MS/MS is as follows：
Chromatographic column：Agilent XDB C18 reversed-phase columns, chromatographic column specification 4.6 × 50mm, 2.7 μm；
Mobile phase：A phases：Aqueous solution, containing 0.1% formic acid, B phases：Methanol；
The gradient elution time：12min；
Gradient elution program：0 → 0.5min, 75%A phase；0.5 → 2min, 75% → 50%A phase；2 → 6min, 50%A
Phase；6 → 7min, 50% → 10%A phase；7 → 9min, 10%A phase；9 → 12min, 10% → 75%A phase；
Flow velocity：0.3mL/min；
Sample size：2μL；
Chromatogram column temperature：30℃；
The Mass Spectrometry Conditions of the LC-MS/MS are as follows：
Ion gun：Electric spray ion source；
Scan mode：Cation scans；
Detection mode：Multiple-reaction monitoring；
Ionizing voltage：5500V；
Atomization gas：50-60psi
Aid in gas：50-60psi
Gas curtain atmospheric pressure：35psi；
Atomization temperature：500-550℃.
Qualitative ion pair, quota ion pair and other mass spectrometry parameters are shown in Table 2.
Qualitative ion pair, quota ion pair and the mass spectral analysis parameter of 2 nine kinds of compounds of table
*：Quota ion
The beneficial effects of the present invention are the plant established based on liquid-liquid extraction-liquid chromatography-tandem mass spectrometry positive ion mode
6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2 in thing grease；3 kinds of flavouring agent vanillic aldehydes, methyl chinese cymbidium
Detection method while element and Ethyl vanillin, sample is after water and acetonitrile carry out solvent extraction, then is aided with ultrasonic extraction, extracts
Liquid carries out Tandem Mass Spectrometry Analysis, the average recovery rate of 9 kinds of compounds exists after the distribution purification of n-hexane liquid liquid under gradient condition
Between 87.4%-94.6%, detection limit：Aflatoxin is 0.06 μ g/kg；Vanillic aldehyde, methyl vanillin and Ethyl vanillin
For 10 μ g/kg.
The present invention is with pre-treatment is simple, sample and solvent usage amount are few, matrix interference is small, analyze speed is fast, sensitivity
High and high repeatability and other advantages, the analysis detection of the invention that can realize aflatoxin and flavouring agent at the same time, greatly improves in addition
The timeliness of inspection, can be suitably used for the quick detection of batch samples, meets routine testing requirements of one's work.
Brief description of the drawings
Fig. 1 is the second order ms figure (qualitative and quota ion selection figure) of vanillic aldehyde of the embodiment of the present invention.
Fig. 2 is the second order ms figure (qualitative and quota ion selection figure) of methyl vanillin of the embodiment of the present invention.
Fig. 3 is the second order ms figure (qualitative and quota ion selection figure) of Ethyl vanillin of the embodiment of the present invention.
Fig. 4 is the second order ms figure (qualitative and quota ion selection figure) of aflatoxin B1 of the embodiment of the present invention.
Fig. 5 is the second order ms figure (qualitative and quota ion selection figure) of aflatoxin B of the embodiment of the present invention 2.
Fig. 6 is the second order ms figure (qualitative and quota ion selection figure) of aflatoxin G 1 of the embodiment of the present invention.
Fig. 7 is the second order ms figure (qualitative and quota ion selection figure) of aflatoxin G of the embodiment of the present invention 2.
Fig. 8 is the second order ms figure (qualitative and quota ion selection figure) of Aflatoxins M1 of the embodiment of the present invention.
Fig. 9 is the second order ms figure (qualitative and quota ion selection figure) of aflatoxin M of the embodiment of the present invention 2.
Figure 10 be corn oil of the embodiment of the present invention in 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and
AFM2；3 kinds of flavouring agent vanillic aldehydes, methyl vanillin and Ethyl vanillin multiple-reaction monitoring (MRM) chromatogram.
Figure 11 be corn oil of the embodiment of the present invention in 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and
AFM2；3 kinds of flavouring agent vanillic aldehydes, methyl vanillin and Ethyl vanillin selection ion stream chromatogram.
Embodiment
To make those skilled in the art more fully understand technical scheme, below in conjunction with the accompanying drawings and following embodiments
Technical scheme is further explained, but not as limiting the scope of the invention.
Embodiment 1
(1) liquid-liquid extraction：1g samples are weighed, add 2mL acetonitriles, vortex oscillation 30s, is ultrasonically treated at 20-25 DEG C
After 10min, supersonic frequency 35Khz, 10000r/min centrifugation 5min, supernatant liquor 1mL is taken, it is to be clean.
(2) liquid liquid distribution purification：In 1mL supernatant liquors add 2mL n-hexanes, vortex oscillation 30s, 10000r/min from
After heart 1min, subnatant is taken, crosses miillpore filter, it is to be analyzed.
(3) standard solution is prepared：First, vanillic aldehyde, methyl vanillin and Ethyl vanillin 0.1g (essences are accurately weighed respectively
Really to 0.0001g), methanol is dissolved and is settled in 100mL volumetric flasks, and 1.0mg/mL standard reserving solutions are made, use dilution in acetonitrile
To 1.0mg/L hybrid standards storing solution 1.Appropriate aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2 are drawn respectively
Standard solution is settled in 10mL volumetric flasks, and 0.1mg/L hybrid standards storing solution 2 is made.Secondly, it is accurate respectively to draw standard storage
Standby liquid 1 and 2 is appropriate, is diluted to bare substrate extracting solution in above-mentioned steps fragrant containing vanillic aldehyde, methyl vanillin and ethyl
Blue element 10ng/mL, 20ng/mL, 40ng/mL, 80ng/mL, 160ng/mL；AFB1 containing aflatoxin, AFB2, AFG1, AFG2,
AFM1 and AFM2 0.1ng/mL, the hybrid standard series of tasks of 0.5ng/mL, 1.0ng/mL, 2.0ng/mL, 5.0ng/mL are molten
Liquid.
(4) qualitative and quantitative analysis：It is analysed to liquid and enters liquid chromatography-tandem mass spectrometry instrument (LC-MS/MS), using more reaction
Monitor (MRM) mode monitoring, quantified by external standard method.The specific test condition of qualitative and quantitative analysis is as follows：
LC-MS/MS chromatographic conditions：Chromatographic column uses Agilent XDB C18 reversed-phase columns, chromatographic column specification for 4.6 ×
50mm, 2.7 μm；Mobile phase is：A phases are aqueous solution (containing 0.1% formic acid), and B phases are methanol；Gradient elution program：0→
0.5min, 75%A phase；0.5 → 2min, 75% → 50%A phase；2 → 6min, 50%A phase；6 → 7min, 50% → 10%A phase；
7 → 9min, 10%A phase；9 → 12min, 10% → 75%A phase.Flow velocity is 0.3mL/min；Sample size is 2 μ L；Chromatogram column temperature
For 30 DEG C.
The Mass Spectrometry Conditions of LC-MS/MS：Ion gun is electric spray ion source；Scan mode scans (ESI+) for cation；Inspection
Survey mode is multiple-reaction monitoring (MRM)；Ionizing voltage (IS) is 5500V；Atomization gas (Gas1) is 50psi；Aid in gas
(Gas2) it is 50psi；Gas curtain atmospheric pressure (CUR) is 35psi；Atomization temperature (TEM) is 500 DEG C.
The present invention carry out chromatographic column selection when, selected respectively Waters HSS T3 columns (2.1mm × 100mm, 2.5
μm), Agilent poroshell 120EC C18 columns (4.6mm × 50mm, 2.7 μm), Kinretex F5 columns (3.0mm ×
50mm, 2.6 μm), Agilent XDB C18 columns (4.6mm × 50mm, 1.8 μm) and Agilent SB C18 columns (2.1mm ×
100mm, 1.8 μm) five kinds of different column packings and different end-blocking chromatographic columns.The result shows that the mobile phase ladder set in our current research
Under the conditions of degree, 9 kinds of compounds have good chromatography retention behavior in five kinds of chromatographic columns, consider each testing compound
Peak shape, response, separating degree and commodity price, it is final to choose Agilent XDB C18 columns (4.6mm × 50mm, 1.8 μm) chromatography
Column.
The present invention has investigated methanol/water system and acetonitrile/water system when carrying out the selection of mobile phase, and basic herein
The upper comparison for carrying out acid modification agent, adds 0.1% formic acid, 0.2% formic acid, 0.1% acetic acid, 0.2% acetic acid in mobile phase.
The result shows that 0.1% formic acid is added in selection in water phase, and when organic phase selects methanol, under condition of gradient elution, Neng Goushi
Existing 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2；3 kinds of flavouring agent vanillic aldehydes, methyl vanillin and second
The optimal baseline separation of base vanillic aldehyde and the collection of optimal mass signal.
The present invention is in the selection of Extraction solvent, because nine kinds of involved compounds are all soluble in methanol, acetonitrile isopolarity
Organic reagent, therefore the common methanol in laboratory and acetonitrile are selected first in sample extraction process as Extraction solvent.Experiment knot
Fruit shows that methanol and acetonitrile can reach more than 85% to the extraction efficiency of nine kinds of compounds, it is contemplated that methanol is to oil sample
The extraction of middle impurity is notable compared with acetonitrile, to reach preferable clean-up effect, present invention determine that acetonitrile is as Extraction solvent.
In addition, researches show that ultrasound contributes to extraction of the acetonitrile to nine kinds of compounds, ultrasonic 1min, 5min, 10min,
15min, 20min and 25min, with the extension of ultrasonic time, extraction recovery increase of the acetonitrile to nine kinds of compounds, the time arrives
During up to more than 10min, extraction recovery does not show significantly to change, present invention determine that the ultrasound assisted extraction time is 10min.
In the embodiment of the present invention, vanillic aldehyde and methyl vanillin are purchased from the USP U.S. purchased from TRC Canada, Ethyl vanillin,
Aspertoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2 are purchased from the SUPELCO U.S., and mentioned reagent purity is both greater than 98%.
(5) result and analysis
A) under selected chromatography and Mass Spectrometry Conditions, the standard that series concentration is measured according to identified plant oil matrix is molten
Liquid, using the concentration of object as abscissa (x), the peak area of chromatographic peak is ordinate (y), carries out regression analysis, the results are shown in Table
3, by table 3 as it can be seen that vanillic aldehyde and Ethyl vanillin are in the range of 10-400 μ g/L, methyl vanillin is in 10-200 μ g/L scopes
Interior, AFB1 and AFG1 are in the range of 0.1-20 μ g/L, and AFB2 is in the range of 0.1-10 μ g/L, and AFG2, AFM1 and AFM2 are in 0.1-8
In the range of μ g/L, there is good linear, correlation coefficient r ＞ 0.997.According to international pure and applied chemistry federation
(IUPAC) to the definition of detection limit, dilute and detect serial mixed standard solution, calculate signal-to-noise ratio (S/N), using S/N=3 as inspection
Rising limit (LOD), using S/N=10 as quantitative limit (LOQ).It is molten that hybrid standard is quantitatively added into the blank sample without target substance
Liquid, is detected after processing, and the LOD of three kinds of flavouring agents is 10 μ g/kg, and the LOQ of method is 35 μ g/kg；Aflatoxin
LOD is 0.06 μ g/kg, and the LOQ of method is 0.2 μ g/kg.
The linear equation of 6 kinds of aflatoxin and 3 kinds of flavouring agents, related coefficient, the range of linearity (n in 3 plant oil matrix of table
=6), detection limit and quantitative limit
B) choose and be free of 6 kinds of aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2；3 kinds of flavouring agent chinese cymbidiums
The plant oil samples of element, methyl vanillin and Ethyl vanillin, the rate of recovery and precision are added according to three concentration levels
Experiment, each level do 6 it is parallel, be measured according to operating procedure as defined in method, investigate the average recovery rate of method, see
Table 4.The result shows that plant oil matrix mark-on average recovery rate is between 87.4%~94.6%, relative standard deviation (RSD) between
1.7%~4.6%, it is satisfied by retention analysis requirement.
The recovery of standard addition and precision (n=6) of 9 kinds of compounds in 4 vegetable oil of table
Claims (2)
1. one kind measures aflatoxin and flavouring agent in vegetable fat at the same time based on liquid-liquid extraction-liquid chromatography-tandem mass spectrometry
Method, it is characterised in that step is as follows：
(1) liquid-liquid extraction：Extraction solvent is added into grease to be measured and blank oil sample, the concussion that is vortexed, ultrasound and centrifugation, obtain
It is to be clean to supernatant liquor；
(2) liquid liquid distribution purification：Purification flux is added in supernatant liquor, vortex oscillation, after centrifugation, takes subnatant, excessively micro-
Hole filter membrane, obtains prepare liquid and bare substrate extracting solution；
(3) standard solution is prepared：First, vanillic aldehyde, methyl vanillin and Ethyl vanillin that mass ratio is 1 are dissolved with methanol
And constant volume, obtain 1.0mg/mL standard reserving solutions, then with dilution in acetonitrile to 1.0mg/L hybrid standards storing solution 1；
Compound concentration is aflatoxin AFB1, AFB2, AFG1, AFG2, AFM1 and AFM2 standard solution of 0.1mg/L respectively,
For hybrid standard storing solution 2；
Hybrid standard storing solution 1 and hybrid standard storing solution 2, mixing are drawn respectively；It is diluted to and is contained with bare substrate extracting solution again
Vanillic aldehyde is respectively 10ng/mL, 20ng/mL, 40ng/mL, 80ng/mL, 160ng/mL, and AFB1 containing aflatoxin is respectively
The hybrid standard series of tasks solution of 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 2.0ng/mL, 5.0ng/mL；
(4) qualitative and quantitative analysis：The prepare liquid that step (2) is obtained enters liquid chromatography-tandem mass spectrometry instrument, is supervised using more reactions
Survey holotype monitoring, quantified by external standard method；
A) qualitative analysis：Using LC-MS/MS methods measure sample and standard working curve is established, if the chromatography detected in prepare liquid
The retention time at peak is consistent with the retention time of respective standard material chromatographic peak, it is allowed to which deviation is less than 2.5%；Further compare
The abundance of the qualitative ion of the close each component of concentration in sample to be tested and standard working solution, deviation are no more than scope as defined in table 1,
Then judge that there are corresponding sample to be tested in oil sample；
With respect to the maximum allowable offset of abundance of ions during 1 qualitative confirmation of table
B) quantitative analysis：Hybrid standard series of tasks solution is measured using LC-MS/MS methods, obtains the color of corresponding standard solution
Spectral peak area, using the concentration of hybrid standard working solution as abscissa, using the peak area of chromatographic peak as ordinate, it is bent to draw standard
Line；Sample to be tested is measured with the same terms again, the chromatographic peak area of sample to be tested is obtained, is obtained according to standard working curve to be measured
The concentration of each component in liquid；The response of each component to be measured is in the linear response range of standard working curve in sample to be tested,
If content goes beyond the scope, sample to be tested is taken to analyze again, then with dilution in acetonitrile to debita spissitudo post analysis；
(5) result calculates：
Calculation formula：
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<mi>X</mi>
<mo>=</mo>
<mfrac>
<mrow>
<mi>c</mi>
<mo>&times;</mo>
<mi>V</mi>
</mrow>
<mi>m</mi>
</mfrac>
<mn>...</mn>
<mrow>
<mo>(</mo>
<mn>1</mn>
<mo>)</mo>
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In formula (1)：
The content of component to be measured in X-oil sample, unit are μ g/kg；
The concentration of each component to be measured in the sample to be tested for c-read from standard working curve, unit is μ g/L；
The quality that m-oil sample weighs, unit g；
V-oil sample solution constant volume, unit mL.
2. according to the method described in claim 1, it is characterized in that, the Liquid Chromatography-Tandem Mass Spectrometry test condition such as
Under：The chromatographic condition of the LC-MS/MS is as follows：
Chromatographic column：Agilent XDB C18 reversed-phase columns, chromatographic column specification 4.6 × 50mm, 2.7 μm；
Mobile phase：A phases：Aqueous solution, containing 0.1% formic acid, B phases：Methanol；
The gradient elution time：12min；
Gradient elution program：0 → 0.5min, 75%A phase；0.5 → 2min, 75% → 50%A phase；2 → 6min, 50%A phase；6
→ 7min, 50% → 10%A phase；7 → 9min, 10%A phase；9 → 12min, 10% → 75%A phase；
Flow velocity：0.3mL/min；
Sample size：2μL；
Chromatogram column temperature：30℃；
The Mass Spectrometry Conditions of the LC-MS/MS are as follows：
Ion gun：Electric spray ion source；
Scan mode：Cation scans；
Detection mode：Multiple-reaction monitoring；
Ionizing voltage：5500V；
Atomization gas：50-60psi
Aid in gas：50-60psi
Gas curtain atmospheric pressure：35psi；
Atomization temperature：500-550℃.
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| CN113075347A (en) * | 2021-04-01 | 2021-07-06 | 广东省农业科学院农业生物基因研究中心 | High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol |
| CN114624341A (en) * | 2020-12-09 | 2022-06-14 | 中国科学院大连化学物理研究所 | Analysis method for simultaneously determining multiple mycotoxins in food |
| CN115006879A (en) * | 2022-06-01 | 2022-09-06 | 郑州大学 | Fiber support liquid-liquid extraction method for grease sample detection, device and application thereof |
| CN115015430A (en) * | 2022-05-26 | 2022-09-06 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Method for detecting aflatoxin in soy sauce |
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| CN116124930A (en) * | 2022-12-27 | 2023-05-16 | 河南工业大学 | Method for determining aflatoxin early-warning indicator averant in high-fat sample matrix |
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| CN110108821A (en) * | 2019-04-22 | 2019-08-09 | 广西壮族自治区疾病预防控制中心 | A kind of dispersive solid-phase extraction material and the preparation method and application thereof |
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| CN114624341B (en) * | 2020-12-09 | 2023-05-30 | 中国科学院大连化学物理研究所 | Analysis method for simultaneously determining multiple mycotoxins in food |
| CN113075347A (en) * | 2021-04-01 | 2021-07-06 | 广东省农业科学院农业生物基因研究中心 | High performance liquid chromatography-triple quadrupole mass spectrometry combined method for rapidly detecting polyphenol |
| WO2022262245A1 (en) * | 2021-06-15 | 2022-12-22 | 浙江海正药业股份有限公司 | Method for analyzing and detecting trace aflatoxin in water-soluble fermented medicament |
| CN115015430B (en) * | 2022-05-26 | 2023-12-12 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Method for detecting aflatoxin in soy sauce |
| CN115015430A (en) * | 2022-05-26 | 2022-09-06 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Method for detecting aflatoxin in soy sauce |
| CN115006879A (en) * | 2022-06-01 | 2022-09-06 | 郑州大学 | Fiber support liquid-liquid extraction method for grease sample detection, device and application thereof |
| CN115006879B (en) * | 2022-06-01 | 2024-04-26 | 郑州大学 | Fiber support liquid-liquid extraction method for detecting grease sample, device and application thereof |
| CN115524434A (en) * | 2022-09-30 | 2022-12-27 | 宁波市疾病预防控制中心 | Universal purification method for measuring various mycotoxins in edible oil |
| CN115524434B (en) * | 2022-09-30 | 2024-01-16 | 宁波市疾病预防控制中心 | Universal purifying method for measuring multiple mycotoxins in edible oil |
| CN116124930B (en) * | 2022-12-27 | 2023-10-20 | 河南工业大学 | Method for determining aflatoxin early-warning indicator averant in high-fat sample matrix |
| CN116124930A (en) * | 2022-12-27 | 2023-05-16 | 河南工业大学 | Method for determining aflatoxin early-warning indicator averant in high-fat sample matrix |
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