CN102692469A - Method for using liquid phase chromatography-tandem mass spectrometry method to determine content of mycotoxin in ginseng - Google Patents
Method for using liquid phase chromatography-tandem mass spectrometry method to determine content of mycotoxin in ginseng Download PDFInfo
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Abstract
The invention discloses a method for using a liquid phase chromatography-tandem mass spectrometry method to determine the content of mycotoxin in ginseng. The method is characterized in that the method comprises the following steps: (1) pretreating a to-be-determined ginseng sample; and (2) determining the content of one or a plurality of mycotoxins in the pretreated ginseng sample through the liquid phase chromatography-tandem mass spectrometry method. The method has the advantages of high sensitivity, high specificity and high accuracy, being capable of being used in determining residues of multiple components of the mycotoxin in the ginseng or similar medical materials.
Description
Technical field
The present invention relates to the assay method of mycotoxin levels in the genseng, be specifically related to adopt the method for mycotoxin levels in liquid chromatography-polyphone mass spectrometric determination genseng.
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 genseng 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 genseng.This method can be used for the residual examination of mycotoxin in the genseng, 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 genseng mycotoxin levels is provided, it is characterized in that, this method comprises the steps:
(1) with the HLB post samples of Ginseng to be measured is carried out pre-service;
(2) content through liquid chromatography-polyphone mass spectrometric determination one or more mycotoxins in pretreated samples of Ginseng.
According to of the present invention one preferred embodiment, said mycotoxin comprises aflatoxin, T-2 toxin, fumonisin B
1, zearalenone, vomitoxin or ochratoxin A; Wherein said aflatoxin comprises AFB
1, AFB
2, AFG
1Or AFG
2
According to of the present invention one preferred embodiment, said HLB post is earlier used methanol-eluted fractions before the pre-service samples of Ginseng, use water elution again.
Preferred embodiment the pre-service of said samples of Ginseng comprises with methanol extraction samples of Ginseng to be measured according to one of the present invention, last HLB post and the step of collecting the solution that flows out the HLB post; Or comprise that with methanol extraction samples of Ginseng to be measured last HLB post is also used methanol-eluted fractions, collects the step of meoh eluate.
Especially preferred embodiment the pre-service of samples of Ginseng comprises: precision takes by weighing the samples of Ginseng powder according to one of the present invention, accurate methanol solution, the sonicated of adding; Centrifugal, filter accurate supernatant, the dilute with water drawn; Shake up, get the HLB post of solution after the dilution,, collect the solution that flows out the HLB post until there being an amount of air to pass through through having handled well; Slowly dry up with nitrogen, the accurate methanol solution that adds makes dissolving, promptly gets; Or using methanol-eluted fractions behind the HLB post on the sample, and collect meoh eluate, after nitrogen slowly dried up, the accurate methanol solution that adds makes dissolving, and was centrifugal, gets supernatant, promptly gets.
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 the C18 post, moving phase by A mutually and the B phase composition, A is methyl alcohol mutually, B is formic acid mutually, the employing 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-48～53 volts.
The inventive method also comprises the standard items drawing standard curve with various fungimycins, and calculates the content of various fungimycins in the samples of Ginseng thus.
The inventive method is for be applied to residual detection and the analysis of mycotoxin multicomponent in the genseng 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 multicomponent of mycotoxin in genseng or the similar medicinal material.
The inventive method is carried out the sample introduction analysis through liquid chromatography-polyphone mass spectrum to samples of Ginseng, detects the residual quantity of multiple mycotoxin in the genseng, and 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 genseng, 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 (1) of negative ion mode;
Fig. 2 is the total ion current figure of the hybrid standard article solution (2) of negative ion mode;
Fig. 3 is the total ion current figure of the hybrid standard article solution (2) of positive ion mode;
Fig. 4 is the total ion current figure of the need testing solution (1) of negative ion mode;
Fig. 5 is the total ion current figure of the need testing solution (2) of negative ion mode;
Fig. 6 is the total ion current figure of the need testing solution (2) of positive ion mode;
Fig. 7 is the total ion current figure that the application of sample of negative ion mode reclaims need testing solution (1);
Fig. 8 is the total ion current figure that the application of sample of negative ion mode reclaims need testing solution (2);
Fig. 9 is the total ion current figure that the application of sample of positive ion mode reclaims need testing solution (2).
Embodiment
Embodiment 1
1, materials and methods
1.1 key instrument and reagent
Aflatoxin, T-2 toxin, fumonisin B
1, zearalenone, vomitoxin or ochratoxin A standard items (U.S. SUPELCO company); Acetonitrile, formic acid, ammonium formate are chromatographically pure.HLB decontaminating column (Waters company).
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
The preparation precision of contrast stock solution takes by weighing AFB1, AFB 2, aflatoxin G 1, AFG 2, T-2 toxin, ochratoxin A, fumonisin B1, zearalenone is vomitted and it is an amount of to tell toxin mark standard items; Add the solution that acetonitrile is mixed with 5mg/L, as mixing the contrast storing solution.
The above-mentioned mixing contrast of the accurate respectively absorption of the preparation of typical curve solution storing solution is an amount of, and the series that is diluted to the said concentration of following table with 50% methyl alcohol is mixed contrast solution.
Table 3, series standard solution concentration table
Other gets the samples of Ginseng powder, and (magnificent space medicinal material company limited provides; Respectively according to " the method check that Chinese pharmacopoeia version appendix in 2010, GB/T5009.118-2008, GB/T23502-2009, SN/T1572-2005, GB/T23504-2009, GB/T23503-2009 describe; Do not detect AFB1, AFB 2, aflatoxin G 1, AFG 2, T-2 toxin, ochratoxin A, fumonisin B 1, zearalenone and vomitoxin) (crossing sieve No. two) 5g; The accurate title, decide; Be operated to " collecting the solution that flows out the HLB post; slowly dry up " according to following " preparation of need testing solution " below method preparation with nitrogen; Add above-mentioned series standard solution 1ml respectively, as series standard curve solution (1).Use 5ml methanol-eluted fractions HLB post subsequently, collect meoh eluate, slowly dry up with nitrogen, the above-mentioned series standard solution 1ml of accurate adding is as series standard curve solution (2).
1.2.4 the preparation of need testing solution
Precision takes by weighing samples of Ginseng powder (magnificent space medicinal material company limited provide) (crossing sieve No. two) 5g, the accurate 70% methanol solution 50ml that adds, and sonicated 30 minutes, centrifugal; Filter, the accurate supernatant 10ml that draws is diluted with water to 20ml; Shake up, the accurate solution 5ml that draws after the dilution, slowly through the HLB that handled well (earlier with methyl alcohol 2ml wash-out; Water 2ml wash-out again) post until there being an amount of air to pass through, is collected the solution that flows out the HLB post; Slowly dry up with nitrogen, the accurate 50% methyl alcohol 1ml solution that adds makes dissolving, as need testing solution (1); Use 5ml methanol-eluted fractions HLB post subsequently, collect meoh eluate, slowly dry up with nitrogen, the accurate 50% methyl alcohol 1ml solution that adds makes dissolving, as need testing solution (2).
2, result
2.1 measure
Accurate respectively above-mentioned series standard curve solution (1) and each 1 μ l of need testing solution (1) of drawing; Inject liquid chromatograph-mass spectrometer; Measure, press calibration curve method and measure the content that calculates vomitoxin, accurate again series standard curve solution (2) and each 1 μ l of need testing solution (2) of drawing; Inject liquid chromatograph-mass spectrometer; Measure, press calibration curve method and measure the content that calculates AFB1, AFB 2, aflatoxin G 1, AFG 2, T-2 toxin, fumonisin B1, ochratoxin A, zearalenone, promptly get.
2.2 calculate
In the formula:
ω---the concentration of every kind of toxin in the sample, μ g/kg;
The concentration of every kind of toxin in ρ---the test solution that from typical curve, draws, ng/ml;
M---sample volume, g.
Do not detect vomitoxin, AFB1, AFB 2, aflatoxin G 1, AFG 2, T-2 toxin, fumonisin B1, ochratoxin A or zearalenone in the above-mentioned samples of Ginseng.
2.3 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
2.4 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
2.5 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 1.3%-3.1% scope, precision is good.
2.6 stability test
Fetch the sample solution of the consistency under the yield test item, every at a distance from sample introduction analysis in 6 hours, the record peak area, the result shows that within 0-12 hour, sample solution is basicly stable.
2.7 average recovery test
Get samples of Ginseng powder 5g, the standard items that add the variable concentrations level respectively are an amount of, and method is operated in accordance with the law under the article processing item in the same old way, calculate recovery rate and corresponding RSD value.Result's (seeing table 6) shows that the result is good for this method recovery test.
Table 6, recovery test (n=9)
Claims (14)
1. be used for measuring the method for genseng mycotoxin levels, it is characterized in that, this method comprises the steps:
(1) with the HLB post samples of Ginseng to be measured is carried out pre-service;
(2) content through liquid chromatography-polyphone mass spectrometric determination one or more mycotoxins in pretreated samples of Ginseng.
2. method according to claim 1 is characterized in that, said mycotoxin is selected from aflatoxin, T-2 toxin, fumonisin B
1, zearalenone, vomitoxin or ochratoxin A.
3. method according to claim 2 is characterized in that said aflatoxin is selected from AFB
1, AFB
2, AFG
1Or AFG
2
4. method according to claim 1 is characterized in that, said HLB post is used methanol-eluted fractions earlier before the pre-service samples of Ginseng, use water elution again.
5. method according to claim 1 is characterized in that, the pre-service of samples of Ginseng to be measured comprises with methanol extraction samples of Ginseng to be measured in the said step (1), last HLB post and the step of collecting the solution that flows out the HLB post; Or comprise that with methanol extraction samples of Ginseng to be measured last HLB post is also used methanol-eluted fractions, collects the step of meoh eluate.
6. method according to claim 1 is characterized in that, the pre-service of samples of Ginseng to be measured comprises in the said step (1): precision takes by weighing the samples of Ginseng powder, the accurate methanol solution that adds; Sonicated, centrifugal, filter the accurate supernatant of drawing; Dilute with water shakes up, and gets the HLB post of solution through having handled well after the dilution, until there being an amount of air to pass through; Collect the solution that flows out the HLB post, dry up with nitrogen, the accurate methanol solution that adds makes dissolving; Or using methanol-eluted fractions behind the HLB post on the sample, and collect meoh eluate, after nitrogen dried up, the accurate methanol solution that adds makes dissolving, and was centrifugal, gets supernatant.
7. 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 C18 post, moving phase is by A phase and B phase composition, and A is methyl alcohol mutually, and B is formic acid mutually, adopts gradient elution.
8. 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-48～53 volts.
9. method according to claim 7 is characterized in that, 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.
10. method according to claim 7 is characterized in that, said C18 post is an ACQUITY UPLC BEH C18 post.
11. method according to claim 7 is characterized in that, wherein the concentration of B phase is 0.01～0.05%.
12. method according to claim 7 is characterized in that, wherein the concentration of B phase is 0.01%.
13. method according to claim 7 is characterized in that, wherein A: the B volume ratio is 5～95%: 95～5%.
14. method according to claim 7 is characterized in that, wherein the flow velocity of moving phase is 0.2～0.4ml/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103344715A (en) * | 2013-06-20 | 2013-10-09 | 中国环境科学研究院 | Method for separation and enrichment of penicillin antibiotics in water |
| CN103543221A (en) * | 2013-09-30 | 2014-01-29 | 王加启 | Method for simultaneously detecting multiple mycotoxins in milk |
| 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 |
| CN104391057A (en) * | 2014-11-24 | 2015-03-04 | 重庆市动物疫病预防控制中心 | Pretreatment kit for detecting ochratoxin A in pig tissue and application of pretreatment kit for detecting ochratoxin A in pig tissue |
| 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 |
| CN107153103A (en) * | 2017-06-26 | 2017-09-12 | 四川省农业科学院分析测试中心 | A kind of method for determining a variety of mycotoxin contents in fresh milk sample |
| 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 |
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| CN111879874A (en) * | 2020-08-04 | 2020-11-03 | 山东中医药大学 | Method for determining aflatoxin content in platycladi seeds |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181853A (en) * | 1976-12-10 | 1980-01-01 | Varian Associates, Inc. | Liquid chromatography system with packed flow cell for improved fluorescence detection |
| CN1645134A (en) * | 2005-01-26 | 2005-07-27 | 上海大学 | Detection for zearalenone |
| CN101109735A (en) * | 2007-05-14 | 2008-01-23 | 劲牌有限公司 | Fluorescence photometry for immune affinity column of aflatoxin in paddy |
| KR20090095177A (en) * | 2008-03-05 | 2009-09-09 | 한국과학기술원 | Method for assaying mycotoxin |
-
2011
- 2011-03-21 CN CN201110067385.XA patent/CN102692469B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181853A (en) * | 1976-12-10 | 1980-01-01 | Varian Associates, Inc. | Liquid chromatography system with packed flow cell for improved fluorescence detection |
| CN1645134A (en) * | 2005-01-26 | 2005-07-27 | 上海大学 | Detection for zearalenone |
| CN101109735A (en) * | 2007-05-14 | 2008-01-23 | 劲牌有限公司 | Fluorescence photometry for immune affinity column of aflatoxin in paddy |
| KR20090095177A (en) * | 2008-03-05 | 2009-09-09 | 한국과학기술원 | Method for assaying mycotoxin |
Non-Patent Citations (8)
Cited By (13)
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| CN103344715A (en) * | 2013-06-20 | 2013-10-09 | 中国环境科学研究院 | Method for separation and enrichment of penicillin antibiotics in water |
| CN103543221A (en) * | 2013-09-30 | 2014-01-29 | 王加启 | Method for simultaneously detecting multiple mycotoxins in milk |
| 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 |
| CN104391057A (en) * | 2014-11-24 | 2015-03-04 | 重庆市动物疫病预防控制中心 | Pretreatment kit for detecting ochratoxin A in pig tissue and application of pretreatment kit for detecting ochratoxin A in pig tissue |
| CN104391057B (en) * | 2014-11-24 | 2016-08-24 | 重庆市动物疫病预防控制中心 | For detecting pretreating reagent box and the application thereof of ochratoxin A in porcine tissue |
| 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 |
| CN107153103A (en) * | 2017-06-26 | 2017-09-12 | 四川省农业科学院分析测试中心 | A kind of method for determining a variety of mycotoxin contents in fresh milk sample |
| 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 |
| CN108426962A (en) * | 2018-05-23 | 2018-08-21 | 华南理工大学 | Method that is a kind of while detecting 7 kinds of typical fungus toxin in fruits and vegetables |
| CN108426962B (en) * | 2018-05-23 | 2021-01-19 | 华南理工大学 | Method for simultaneously detecting 7 typical mycotoxins in fruits and vegetables |
| CN109828072A (en) * | 2019-02-21 | 2019-05-31 | 安徽润安信科检测科技有限公司 | A kind of method that ultra performance liquid chromatography-triple quadrupole bar tandem mass spectrometer detects 16 kinds of biotoxins in liquor-making raw material simultaneously |
| CN111879874A (en) * | 2020-08-04 | 2020-11-03 | 山东中医药大学 | Method for determining aflatoxin content in platycladi seeds |
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