CN102654490A - Method for measuring content of mycotoxins in araliaceae plants by liquid chromatography-tandem mass spectrometry - Google Patents
Method for measuring content of mycotoxins in araliaceae plants by liquid chromatography-tandem mass spectrometry Download PDFInfo
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Abstract
The invention discloses a method for measuring the content of mycotoxins in araliaceae plants by liquid chromatography-tandem mass spectrometry, comprising the following steps of: (1) preprocessing an araliaceae plant sample to be measured by a solid-phase extraction column; and (2) measuring the content of one or more mycotoxins in the preprocessed araliaceae plant sample through the liquid chromatography-tandem mass spectrometry. The measurement method is high in sensitivity, good in specificity and good in accuracy, and applied to measurement of multiple component residuals of the mycotoxins in the araliaceae plants.
Description
Technical field
The present invention relates to the assay method of mycotoxin levels in the Araliaceae, be specifically related to adopt the method for mycotoxin levels in liquid chromatography-polyphone mass spectrometric determination Araliaceae.
Background technology
Mycotoxin (Mycotoxin) is also claimed mycotoxin, is mycetogenetic secondary metabolite, generally has strong toxicity simultaneously and pollutes the high characteristics of frequency.Owing to the parasitism of fungi and the generation of mycotoxin, have a strong impact on the output of crops, reduce agricultural product and feed quality, cause the tremendous economic loss.The human or animal takes in farming, the livestock products that polluted by mycotoxin, or can cause multiple toxicity symptom through suction and skin contact mycotoxin.As cause unreal, emetic, haemorrhage, dermatitis, nervous centralis is impaired, even dead.Animal experiment and EPDML investigation result also confirm; Many mycotoxins also can accumulate the back in vivo and produce carcinogenic, teratogenesis, mutagenesis, parahormone and poison; Aleucemia etc.; Body is caused permanent lesion (referring to Zhang Yibing etc., the check and analysis of mycotoxin [M] Beijing in the agricultural product: Chemical Industry Press, 2006).
The mycotoxin that research is at present paid close attention to mainly concentrates on aflatoxin (aflatoxin), ochratoxin (OA), vomitoxin (DON), fumonisin (FUM), zearalenone (ZEN), T-2 toxin and patulin (PAT) etc.Along with further investigation to mycotoxin harm; The public recognizes the serious threat that it causes social economy and human health gradually; Strictness has been set in great concern, particularly developed country such as the European Union and the U.S. especially to this regulation of limiting the quantity of has also all been given to the distribution and the detection of mycotoxin in the drug and food by national governments.The food aspect; China put into effect in succession much statutory standards about mycotoxin (referring to mycotoxin in the GB2715-2005 food limit the quantity of [S] and GB2761-2005 food in mycotoxin limit the quantity of [S]); But at medicine field; Except that Chinese Pharmacopoeia has recorded examination of aflatoxin method (referring to The People's Republic of China's pharmacopeia version [S] in 2010), still do not have other standards and put into effect.And existing food standard is to single mycotoxin and detects, and does not still have and detects the residual standard appearance of multicomponent simultaneously.
Therefore, be badly in need of the particularly residual efficient measurement method of mycotoxin multicomponent in the Araliaceae of exploitation medicine.
Summary of the invention
In view of the above-mentioned defective of prior art, the present invention provides a kind of method that adopts mycotoxin levels in the liquid chromatography tandom mass spectrometry determination Araliaceae.This method can be used for the residual examination of mycotoxin in the Araliaceae, and the standard of mycotoxin provides technical service in the medicine in order to draft.
The present invention realizes through following technical scheme:
A kind of method that is used for measuring the Araliaceae mycotoxin levels is provided, it is characterized in that, this method comprises the steps:
(1) with solid-phase extraction column Araliaceae sample to be measured is carried out pre-service;
(2) content through liquid chromatography-polyphone mass spectrometric determination one or more mycotoxins in pretreated Araliaceae sample.
According to of the present invention one preferred embodiment, the inventive method is used for measuring the content of the multiple mycotoxin of Araliaceae sample.
According to of the present invention one preferred embodiment, said Araliaceae be genseng, American Ginseng,, panax japonicus or pseudo-ginseng ginseng, be preferably genseng especially.
According to of the present invention one preferred embodiment, said mycotoxin comprises aflatoxin, zearalenone, vomitoxin or T-2 toxin; Wherein said aflatoxin comprises AFB
1, AFB
2, AFG
1Or AFG
2
According to of the present invention one preferred embodiment, said Araliaceae The pretreatment comprises the step with solid-phase extraction column Mycosep 226 multiple function purifying Araliaceae samples.
According to a preferred embodiment of the present invention, said Araliaceae The pretreatment comprises with acetonitrile extracts the step that the Araliaceae sample also passes through Mycosep 226 multiple functions.
According to of the present invention one especially preferred embodiment, the Araliaceae The pretreatment comprises: take by weighing the Araliaceae sample powder, add acetonitrile; Stir, centrifugal, filter; Filtrating is got supernatant, drying through multifunctional purifying post (Mycosep 226); Add methyl alcohol-ammonium formate solution and make dissolving, centrifugal, get supernatant.
According to of the present invention one preferred embodiment; The chromatographic condition of liquid chromatography in the said step (2)-polyphone mass spectroscopy is: adopt octadecyl silane post (C18 post), moving phase is by A phase and B phase composition, and A is 100% methyl alcohol mutually; B is formic acid mutually, adopts gradient elution.
Preferably, the particle diameter of said C18 post is 1.7～5 μ m, and column internal diameter 2.1～4.6mm, column length are 5～10cm, more preferably ACQUITY UPLC BEH C18 post; The concentration of B phase is 0.01～0.05%, preferred 0.01% (volume); A: the B volume ratio is 5～95%: 95～5%, and preferable flow rate is 0.2～0.4ml/min, preferred 0.3ml/min.
According to of the present invention one preferred embodiment; The mass spectrum condition of liquid chromatography in the said step (2)-polyphone mass spectroscopy is: adopt electric spray ion source; Adopt the negative ions pattern to carry out data acquisition, go bunch voltage for-100～120 volts, collide the pond energy and be-39～50 volts.
The inventive method also comprises the standard items drawing standard curve with various fungimycins, and calculates the content of fungimycin in the Araliaceae thus.
The inventive method is for be applied to residual detection and the analysis of mycotoxin multicomponent in the Araliaceae first.The inventive method can effectively be got rid of interference, guarantee the stable of determinand in the residual detection of the multicomponent of medicine mycotoxin.This determination and analysis method is highly sensitive, specificity is strong, accuracy good, can be used for the residual mensuration of the multicomponent of mycotoxin in the Araliaceae.
The inventive method is carried out the sample introduction analysis through liquid chromatography-polyphone mass spectrum to the Araliaceae sample; Detect the residual quantity of multiple mycotoxin in the Araliaceae; Analysis cost is low, reduced false positive again simultaneously, improved the accuracy of measuring, and stronger practicality is arranged.This method has great importance to the residual detection of mycotoxin multicomponent in the Araliaceae, and gordian techniquies such as new drug are had good directive significance, can be applicable to many aspects such as new drug development Quality Control.This method can effectively be applied to the formulation of national standard, the research and development of enterprise's new drug, the lifting of enterprise's existing product quality control method.
Description of drawings
Fig. 1 is the total ion current figure of the hybrid standard article solution of negative ion mode;
Fig. 2 is the total ion current figure of the hybrid standard article solution of positive ion mode;
Fig. 3 is the total ion current figure of the need testing solution of negative ion mode;
Fig. 4 is the total ion current figure of the need testing solution of positive ion mode;
Fig. 5 is the total ion current figure that the application of sample of negative ion mode reclaims need testing solution;
Fig. 6 is the total ion current figure that the application of sample of positive ion mode reclaims need testing solution.
Embodiment
Except as otherwise noted, all proportions, percentage composition and umber by volume all among the present invention.
1, materials and methods
1.1 key instrument and reagent
Aflatoxin, vomitoxin, zearalenone, T-2 toxin standard items (U.S. SUPELCO company); Acetonitrile, formic acid, ammonium formate are chromatographically pure.Mycosep 226 multifunctional purifying posts (Romer company).Genseng is purchased China's space medicinal material company limited in Shanghai, the place of production: Jilin, lot number: 20040404.
1.2 experimental technique
1.2.1 chromatographic condition
ACQUITY UPLC BEH C18 (1.7 μ m, 2.1 * 100mm); With 100% methyl alcohol is the mobile phase A phase, is the Mobile phase B phase with 0.01% formic acid, flow velocity 0.3ml/min; According to the form below carries out gradient elution:
Table 1, eluent gradient
1.2.2 mass spectrum condition
Ion gun is ESI source, electro-spray ionization source; Kapillary goes mass spectrum parameters such as a bunch voltage, collision pond energy to see table 2.
Table 2, mass spectrum parameter list
1.2.3 the preparation of standard solution
Precision takes by weighing AFB
1, AFB
2, AFG
1, AFG
2, T-2 toxin and zearalenone standard items are an amount of, add the solution that acetonitrile is mixed with 1mg/L, as standard reserving solution.It is an amount of that precision takes by weighing the vomitoxin standard items in addition, adds the storing solution that acetonitrile is mixed with 5mg/L.
The above-mentioned storing solution of accurate respectively absorption is an amount of, is diluted to the series standard solution of the said concentration of following table with blank matrix solution.
Table 3, series standard solution concentration table
1.2.4 the preparation of need testing solution
Precision takes by weighing samples of Ginseng powder (crossing sieve No. two) 10g, puts in the homogenate cup acetonitrile 40ml of accurate adding 84%, high-speed stirred 2 minutes; Add acetonitrile 40ml again, high-speed stirred 1 minute, centrifugal, filter; Filtrating is through multifunctional purifying post (Mycosep 226), and precision is measured supernatant 5ml, and after nitrogen slowly dried up, the accurate 1ml methyl alcohol-10mmol/L ammonium formate solution (1: 1) that adds made dissolving; Centrifugal, get supernatant, promptly get.
2, result
2.1 measure
Above-mentioned each the standard solution sample introduction 1 μ l of accurate respectively absorption analyzes the drawing standard curve according to above-mentioned condition sample introduction.The accurate in addition need testing solution 1 μ l that draws analyzes according to above-mentioned condition sample introduction, reads corresponding amount from typical curve, calculates, and promptly gets.
Computing formula:
In the formula:
X (μ g/Kg)---the content of composition to be measured in the sample;
A (ng/mL)---the concentration of composition to be measured in the need testing solution;
M (g)---the sample weighting amount of sample.
The result shows, does not detect above-mentioned seven kinds of mycotoxins in the sample.
2.2 linear relationship
Accurate each the 1 μ l of above-mentioned series standard solution that draws, each component chromatographic peak area to be measured is write down in the sample introduction analysis, is horizontal ordinate (X) with sample introduction concentration, and peak area is ordinate (Y), carries out regretional analysis, and result's (seeing table 4) shows that each component lines sexual intercourse is good.
Table 4, regression equation and related coefficient
2.3 detectability
Measuring the signal to noise ratio (S/N ratio) of low concentration average recovery solution, is 3: 1 computing method detectabilities (seeing table 5) with signal to noise ratio (S/N ratio), and the result shows that this method detectability is far below the limit standard of present food service industry.
Table 5, detectability
2.4 precision test
Get matrix standard solution 3, continuous sample introduction 6 times, the record peak area, the result shows that the RSD value of 6 sample introduction peak areas of above-mentioned seven kinds of compositions is in the 1.5%-4.4% scope, precision is good.
2.5 average recovery test
Get samples of Ginseng powder 10g, the standard items that add the variable concentrations level respectively are an amount of, operate calculate recovery rate and corresponding RSD value according to method under " preparation of need testing solution " item in accordance with the law.Result's (seeing table 6) shows that the result is good for this method recovery test.
Table 6, recovery test (n=6)
2.6 stability test
Fetch the sample solution of consistency under the yield item, every at a distance from sample introduction analysis in 5 hours, the record peak area, the result shows that within 0～20 hour, sample solution is basicly stable.
Claims (16)
1. be used for measuring the method for Araliaceae mycotoxin levels, it is characterized in that, this method comprises the steps:
(1) with solid-phase extraction column Araliaceae sample to be measured is carried out pre-service;
(2) content through liquid chromatography-polyphone mass spectrometric determination one or more mycotoxins in pretreated Araliaceae sample.
2. method according to claim 1 is characterized in that this method comprises the steps:
(1) with solid-phase extraction column Araliaceae sample to be measured is carried out pre-service;
(2) content through liquid chromatography-polyphone mass spectrometric determination multiple mycotoxin in pretreated Araliaceae sample.
3. method according to claim 3 is characterized in that, said Araliaceae is genseng, American Ginseng, panax japonicus or pseudo-ginseng ginseng.
4. method according to claim 3 is characterized in that, said Araliaceae is a genseng.
5. method according to claim 1 is characterized in that, said mycotoxin is selected from aflatoxin, zearalenone, vomitoxin or T-2 toxin.
6. method according to claim 5 is characterized in that said aflatoxin is selected from AFB
1, AFB
2, AFG
1Or AFG
2
7. method according to claim 1 is characterized in that, the solid-phase extraction column described in the said step (1) is Mycosep 226 multiple functions.
8. according to claim 1 or 7 described methods, it is characterized in that the Araliaceae The pretreatment comprises the step of also passing through Mycosep 226 multiple functions with acetonitrile extraction Araliaceae sample in the said step (1).
9. method according to claim 1 is characterized in that, the Araliaceae The pretreatment may further comprise the steps in the said step (1): take by weighing the Araliaceae sample powder, add acetonitrile; Stir, centrifugal, filter; Filtrating is got supernatant, drying through Mycosep 226 multiple functions; Add methyl alcohol-ammonium formate solution and make dissolving, centrifugal, get supernatant.
10. method according to claim 1 is characterized in that, the chromatographic condition of liquid chromatography in the said step (2)-polyphone mass spectroscopy is: adopt the octadecyl silane post; Moving phase is by A phase and B phase composition; A is methyl alcohol mutually, and B is formic acid mutually, adopts gradient elution.
11. method according to claim 1; It is characterized in that; The mass spectrum condition of liquid chromatography in the said step (2)-polyphone mass spectroscopy is: adopt electric spray ion source, adopt the negative ions pattern to carry out data acquisition, go bunch voltage for-100～120 volts, collide the pond energy and be-39～50 volts.
12. method according to claim 10 is characterized in that, the particle diameter of said octadecyl silane post is 1.7～5 μ m, and column internal diameter 2.1～4.6mm, column length are 5～10cm.
13. method according to claim 10 is characterized in that, wherein the concentration of B phase is 0.01～0.05%.
14. method according to claim 10 is characterized in that, wherein the concentration of B phase is 0.01%.
15. method according to claim 10 is characterized in that, wherein A: the B volume ratio is 5～95%: 95～5%.
16. method according to claim 10 is characterized in that, wherein the flow velocity of moving phase is 0.2～0.4ml/min, preferred 0.3ml/min.
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| CN103954714A (en) * | 2014-01-03 | 2014-07-30 | 南通市产品质量监督检验所 | Method for determination of aflatoxin |
| CN104237367A (en) * | 2014-09-09 | 2014-12-24 | 武汉品生科技有限公司 | Kit applied to small molecular qualitative and quantitative analysis and detection and high-throughout screening of microbial culture solution sample and preparation method of kit |
| CN105891373A (en) * | 2016-06-12 | 2016-08-24 | 浙江大学 | Method for detecting various kinds of fungaltoxin in traditional Chinese medicine injection simultaneously |
| CN107085063A (en) * | 2017-05-26 | 2017-08-22 | 上海市食品药品检验所 | A kind of analysis method of mycotoxin in medicine-food two-purpose kind subclass Chinese medicine |
| CN107860858A (en) * | 2017-11-01 | 2018-03-30 | 上海市食品药品检验所 | A kind of method for high-flux analysis of mycotoxin in plant medicine material |
| CN108107118A (en) * | 2016-11-24 | 2018-06-01 | 天士力医药集团股份有限公司 | The detection method of 9 kinds of mycotoxins in a kind of Cassia obtusifolia L |
| CN111707753A (en) * | 2020-06-24 | 2020-09-25 | 安徽农业大学 | Detection method of wheat scab grain ZEN toxin |
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| CN114062571A (en) * | 2021-11-15 | 2022-02-18 | 厦门大学 | Method for detecting mycotoxin in aquaculture water |
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| CN103954714A (en) * | 2014-01-03 | 2014-07-30 | 南通市产品质量监督检验所 | Method for determination of aflatoxin |
| CN103954714B (en) * | 2014-01-03 | 2016-03-30 | 南通市产品质量监督检验所 | A kind of assay method of aflatoxin |
| CN103713065B (en) * | 2014-01-06 | 2015-09-16 | 上海市农业科学院 | A kind of method simultaneously detecting multiple mycotoxin |
| CN103713065A (en) * | 2014-01-06 | 2014-04-09 | 上海市农业科学院 | Method for simultaneously detecting various fungaltoxins |
| CN104237367A (en) * | 2014-09-09 | 2014-12-24 | 武汉品生科技有限公司 | Kit applied to small molecular qualitative and quantitative analysis and detection and high-throughout screening of microbial culture solution sample and preparation method of kit |
| CN105891373A (en) * | 2016-06-12 | 2016-08-24 | 浙江大学 | Method for detecting various kinds of fungaltoxin in traditional Chinese medicine injection simultaneously |
| CN108107118A (en) * | 2016-11-24 | 2018-06-01 | 天士力医药集团股份有限公司 | The detection method of 9 kinds of mycotoxins in a kind of Cassia obtusifolia L |
| CN107085063A (en) * | 2017-05-26 | 2017-08-22 | 上海市食品药品检验所 | A kind of analysis method of mycotoxin in medicine-food two-purpose kind subclass Chinese medicine |
| CN107860858A (en) * | 2017-11-01 | 2018-03-30 | 上海市食品药品检验所 | A kind of method for high-flux analysis of mycotoxin in plant medicine material |
| CN112920900A (en) * | 2019-12-06 | 2021-06-08 | 中国科学院大连化学物理研究所 | Method for preparing zearalenone in chromatographic degreasing |
| CN111707753A (en) * | 2020-06-24 | 2020-09-25 | 安徽农业大学 | Detection method of wheat scab grain ZEN toxin |
| CN111879874A (en) * | 2020-08-04 | 2020-11-03 | 山东中医药大学 | Method for determining aflatoxin content in platycladi seeds |
| CN114062571A (en) * | 2021-11-15 | 2022-02-18 | 厦门大学 | Method for detecting mycotoxin in aquaculture water |
| CN114062571B (en) * | 2021-11-15 | 2022-08-02 | 厦门大学 | Method for detecting mycotoxin in aquaculture water |
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