CN103822814A - QuEChERS extraction method for poisonous substance extraction and application of QuEChERS extraction method - Google Patents
QuEChERS extraction method for poisonous substance extraction and application of QuEChERS extraction method Download PDFInfo
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Abstract
The invention relates to a QuEChERS extraction method for poisonous substance extraction, which is especially suitable for extracting unknown poisonous substances in food poisoning samples. The scheme is that the extraction method comprises the following steps: at first, extracting homogenized or mixed samples with acidiferous acetonitrile or Na2 EDTA to obtain extract liquor; adding NaC1 and Na2SO4 in the extract liquor, and mixing to obtain mixed liquor; carrying out supersonic centrifuge on the mixed liquor to obtain supernate, enabling the supernate to be subjected to C18 and anhydrous sodium sulfate purification to obtain an extracting solution, and then detecting and analyzing the extracting solution. The extraction method and application are suitable for various different matrixes: pork, pork liver, milk, eggs, fruits, vegetables, gastric juice, blood and urine, are high in recovery rate and quick and reliable to test, are used for quickly screening the actual poisoning samples, and facilitate the timely treatment and criminal investigation on poisoned personnel.
Description
Technical field
The present invention relates to a kind of sample-pretreating method and application thereof, be specially a kind of QuEChERS extracting method extracting for noxious material, be adapted to especially the extraction of unknown poisonous substance in Food Poisoning Samples, realize the rapid screening of food poisoning.
Background technology
QuEChERS (abbreviation of Quick, Easy, Cheap, Effective, Rugged and Safe) method is the quick pretreatment method growing up in recent years, can facilitate, economical, from food substrate, target compound is extracted rapidly.The most original QuEChERS method does not have buffer salt, only have MgSO4 and NaCl, the QuEChERS method of recommendation has in the world at present: the usage in the EN15662 of European Union method and AOAC, EN15662 and AOAC official 2007.01 method improvements the most original method, in extraction step, add buffer salt, this can expand target compound scope, these two methods mainly for matrix be fruit and vegetable, the target compound of measuring is mainly agricultural chemicals, wherein QuEChERS method is expressed as: the filler of extracting tube is 4g MgSO4, 1g NaCl, 1g sodium citrate, 0.5g DisodiumHydrogen Citrate (EN15662), 6gMgSO4, 1.5g sodium acetate (AOAC2007.01 method), the filler of purification pipe optionally adds according to the number of the fatty amount of matrix and pigment: 150mg PSA or C18, or graphitized carbon, with 900mg MgSO4.
QuEChERS method generally comprises two steps: the one, and organic solvent extraction, the 2nd, purify supernatant.The conventional acetonitrile of QuEChERS, for extracting solution, although the solubleness of fat in acetonitrile is not high, still has a considerable amount of fat to be total to extract and exists in extract, this purification method that just need to improve QuEChERS is to adapt to high fat content matrix.Conventional purifying adsorbent comprises: N-propyl group ethylenediamine filler (primary secondary amine, PSA), Graphon (graphitised carbon black, and C18 GCB), three kinds of fillers can adapt to different substrates and purify demand, can be used alone, also can be used in conjunction with.In addition, QuEChERS buffered saline solution is also the fine selection of extracting, and it can take into account the pH value of different compounds, especially good to the extraction effect of pH sensitive compound.Can say, although the extraction and cleaning step of QuEChERS method is simple, need researcher constantly to adjust according to experiment process.
The method is mainly used in the analysis of fruits and vegetables Pesticide Residues at present, also there is small part to be applied to quinolones, sulfamido, benzimidazole, the antibiotic detection of veterinary drugs in food of Avermectins in the animal food matrix such as milk, muscle, egg, liver simultaneously, but because veterinary drug kind is various, character is different, brings certain challenge to multinomial retention analysis testing.Extract aspect, (the Journal of Chromatography A such as Lombardo-Agui, 2011,1218 (30): 4966-4971) based on EN15662 method, the acetonitrile that uses the NaH2PO4 buffer solution of pH7.0 and contain 5% formic acid, as extractant, is analyzed the QNS in milk.Zhang Yi etc. (chromatogram, 2011,29 (6): 523-534) people uses acidifying ethyl acetate as the hormone medicine extracting in solvent analysis feed.The selection aspect of adsorbent, the people such as Stubbings (Journal of Chromatography A, 2008,1205 (1): 10-16) utilize NH2 adsorbent to purify chicken and chicken gizzard sample.Dong waits (Chinese Journal of Health Laboratory Technology, 2008,18 (1): 26-28) quietly and selects C18, PSA and aluminium oxide as cleanser.In addition, the QuEChERS method of some novelties is progressively developed, (the Analytical and Bioanalytical Chemistry such as Vidal, 2010,397 (7): 2777-2790) while analyzing milk sample, only use the extraction step in QuEChERS, after extraction, directly analyze by LC-MS/MS, obtain desirable result; (the Journal of Separation Science such as Karageorgou, 2011,34 (15): 1893-1901) in the time analyzing Penicillin in Milk, innovatively hydrophilic lipophilic solid phase extraction filler Strata-X is combined with MgSO4, PSA, C18 adsorbent, disperses Solid-Phase Extraction to complete pretreatment process by a step.
Present stage, QuEChERS method mainly concentrates on the extraction and purification methods of small amount compound in single-matrix, due to its pretreatment process and outstanding extraction efficiency quickly and easily, researcher is by improve to adapt to multi-component needs that detect in different substrates simultaneously to QuEChERS method, design and develop a kind of can be from animality food substrate and bio-matrix rapid extraction opposed polarity compound pre-treating method and to be applied to rapid screening detection be very necessary.
The noxious material of food poisoning generally includes: macrolides, quinolones, sulfamido, Avermectins, benzopyrazoles class, cephalo-type, blocking agent, sedative, Tetracyclines, adrenin, people's medication, rat poison, organophosphorus pesticide, herbicide, killing acarus and bacteria agent, pesticide and veterinary drug class etc., method of the present invention can be extracted common food poisoning material, matrix is not particularly limited, not only be adapted to fruit and vegetable matrix, also comprise pork, pork liver, egg, the matrix of the high protein such as milk, also be applicable to biological sample matrix simultaneously, as serum, urine, gastric juice etc., it is a kind of pre-treating method of the rapid screening of poisoning by food.
Summary of the invention
The object of this invention is to provide a kind of quick, easy, general pre-treating method, can carry out the rapid extraction of multiple noxious material, simultaneous adaptation is in multiple different substrates: pork, pork liver, milk, egg, fruit, vegetables, gastric juice, blood, urine.
Technical scheme of the present invention is to provide a kind of QuEChERS extracting method extracting for noxious material, first, with extracting containing sour acetonitrile and the sample of disodium ethylene diamine tetraacetate (Na2EDTA) to homogenate or after mixing, obtains extract; In described extract, add sodium chloride (NaCl) and anhydrous sodium sulfate (Na2SO4), mix, obtain mixed liquor; By ultrasonic described mixed liquor centrifugal after, gained supernatant purifies through C18 and anhydrous sodium sulfate, obtain extract, then extract is detected to analysis, the object that wherein adds disodium ethylene diamine tetraacetate is the extraction efficiency that guarantees the materials such as antibiotics, the object that adds sodium chloride is to be more conducive to water layer and acetonitrile layer separately, and the object that adds anhydrous sodium sulfate is for water suction, detects that to analyze be to adopt sewage sludge to detect analysis.
The concrete steps of QuEChERS extracting method of extracting for noxious material comprise: (1) contains the acetonitrile of 1.0% (v/v) formic acid and 0.08～0.12g disodium ethylene diamine tetraacetate with 9～11mL and the equal slurry samples of 2.0g or 2.0ml are mixed to fluid sample extracts, and obtains extract; (2) in described extract, add 0.8～1.2g sodium chloride and 3.5～4.5g anhydrous sodium sulfate, mix, obtain mixed liquor; (3) by ultrasonic described mixed liquor centrifugal after, get gained supernatant 6ml, add 140～160mg C18 and 850～950mg anhydrous sodium sulfate to purify, obtain extract, then extract is detected to analysis.
Particularly preferably be, the QuEChERS extracting method concrete steps of extracting for noxious material comprise: take the equal slurry samples of 2.0g or 2.0ml and mix fluid sample, be placed in centrifuge tube, in centrifuge tube, add 10mL to contain acetonitrile solution and the 0.1gNa2EDTA of 1.0% (v/v) formic acid, shake 1min, then add 1.0g sodium chloride and 4.0g anhydrous sodium sulfate, vortex mixes 15s, ultrasonic 15min, with the centrifugal 5min of 9000r/min, gets supernatant for subsequent use; Separately get 015mL centrifuge tube, add 900mg anhydrous sodium sulfate, 150mg
dSC-18 adsorbent, moves into aforementioned supernatant 6mL, concussion 1min, and the centrifugal 5min of 9000r/min, gets supernatant 1mL for detection of analysis.
The present invention also provides a kind of application of the QuEChERS extracting method extracting for noxious material, and it is mainly used in the rapid screening of food poisoning.
By method of the present invention to pork, pork liver, milk, egg, fruit, vegetables, gastric juice, blood, in these 9 kinds of matrix of urine more than 300 are planted representative toxic compounds and have been carried out sample preparation, and adopt sewage sludge analysis, the recovery is high, mainly concentrate on 70%-120%, wherein toxic compounds mainly comprises macrolides, quinolones, sulfamido, Avermectins, benzopyrazoles class, cephalo-type, blocking agent, sedative, Tetracyclines, adrenin, people's medication, rat poison, organophosphorus pesticide, herbicide, killing acarus and bacteria agent, pesticide and veterinary drug class and great majority food poisoning matrix.
Simple, quick, the universal pre-treating method of setting up by the present invention, for food poisoning, can process fast detection, to obtain reliable results, be used in particular for the rapid screening of actual Poisoned Samples, be conducive to poisoning personnel's timely treatment and criminal investigation work etc.
Accompanying drawing explanation
Fig. 1 illustrates the recovery statistical graph of five kinds of different noxious materials in nine kinds of matrix
Embodiment
Experiment instrument and reagent: Ultra Performance Liquid Chromatography-level Four bar/time of-flight mass spectrometer system (U.S., Waters company); Analytical balance: sensibility reciprocal 0.01g; Eddy mixer; Ultrasonic cleaner; High speed freezing centrifuge; 50mL and 15mL centrifuge tube; The brown volumetric flask of 10mL; PSA, C18, GCB, anhydrous sodium sulfate; Na2EDTA; The organic solvents such as methyl alcohol, water, acetonitrile, acetone, chloroform, methylene chloride, formic acid, ammoniacal liquor, dimethyl formamide, pyridine, correcting fluid LEK, sodium formate.
Conventionally the compound that causes food poisoning is a lot, and the present invention has determined common are and poisons compound and it is extracted, and detects, and particular compound title sees the following form shown in 1:
Table 1 toxic compounds kind and title thereof
The recovery test of 1 five kinds of different noxious materials of embodiment in nine kinds of matrix
Get respectively five parts in milk, liver, pork, egg, fruit, vegetables, gastric juice, blood, these nine kinds of samples of urine, in five kinds of samples of every kind of matrix, add respectively noxious material Orbifloxacin, Lomefloxacin, Pefloxacin, Ofloxacin, Danofloxacin, above each sample is extracted with QuEChERS extracting method of the present invention respectively, and adopt sewage sludge to detect analysis, the recovery sees the following form shown in 2, and wherein milk, liver, pork, egg are commercially available sample; Fruit is the potpourri of apple, pears, orange, grape, dragon fruit; Vegetables are the potpourri of Chinese cabbage, little rape, radish, wormwood artemisia stalk; Gastric juice is simulated gastric fluid, and main proportioning is: 2g sodium chloride, and 3.2g pepsin, the hydrochloric acid of 7mL36.5% adds water to 1000mL; Urine and serum are urine and the serum of Healthy People, the statistical graph of making according to table 3 as shown in Figure 1, except urine matrix, Orbifloxacin, Lomefloxacin, Pefloxacin, Ofloxacin, the recovery of Danofloxacin in milk, liver, pork, egg, fruit, vegetables, gastric juice, blood are all more than 70%; In urine matrix, the recovery of Orbifloxacin, Lomefloxacin is higher, the recovery of Ofloxacin, Ofloxacin, Danofloxacin is minimum also 46.80%, as can be seen here, QuEChERS extracting method of the present invention is high to the extraction efficiency of poisonous substance, and the extraction used time of every kind of sample is 20min, extract fast, for the fast detecting of the unknown food poisoning provides a kind of reliable screening pre-treating method.
The recovery of five kinds of materials of table 2 in nine kinds of matrix
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (6)
1. the QuEChERS extracting method extracting for noxious material, is characterized in that, comprising: (1), with extracting containing sour acetonitrile and the sample of disodium ethylene diamine tetraacetate to homogenate or after mixing, obtains extract; (2) in described extract, add sodium chloride and anhydrous sodium sulfate, mix, obtain mixed liquor; (3) by ultrasonic described mixed liquor centrifugal after, gained supernatant purifies through C18 and anhydrous sodium sulfate, obtains extract, then extract is detected to analysis.
2. a kind of QuEChERS extracting method extracting for noxious material according to claim 1, is characterized in that, is the acetonitrile containing 1% formic acid containing sour acetonitrile.
3. a kind of QuEChERS extracting method extracting for noxious material according to claim 2, it is characterized in that, method comprises: (1) mixes fluid sample containing the acetonitrile of 1.0% (v/v) formic acid and 0.08～0.12g disodium ethylene diamine tetraacetate to the equal slurry samples of 2.0g or 2.0ml with 9～11mL and extracts, and obtains extract; (2) in described extract, add 0.8～1.2g sodium chloride and the anhydrous sodium sulfate that is greater than 4g, wherein anhydrous sodium sulfate addition, for making solution to occurring without caking phenomenon, mixes, and obtains mixed liquor; (3) by ultrasonic described mixed liquor centrifugal after, get gained supernatant 6ml, add 140～160mg C18 and 850～950mg anhydrous sodium sulfate to purify, obtain extract, then extract is detected to analysis.
4. a kind of QuEChERS extracting method extracting for noxious material according to claim 3, it is characterized in that, take the equal slurry samples of 2.0g or 2.0ml and mix fluid sample, be placed in centrifuge tube, in centrifuge tube, add 10mL to contain acetonitrile solution and the 0.1g Na2EDTA of 1.0% (v/v) formic acid, concussion 1min, add 1.0g sodium chloride and the anhydrous sodium sulfate that is greater than 4.0g, vortex mixes 15s, ultrasonic 15min again, with the centrifugal 5min of 9000r/min, get supernatant for subsequent use; Separately get a 15mL centrifuge tube, add 900mg anhydrous sodium sulfate, 150mg
dSC-18 adsorbent, moves into described supernatant 6mL, concussion 1min, and the centrifugal 5min of 9000r/min, gets supernatant 1mL for detection of analysis.
5. according to the arbitrary described a kind of QuEChERS extracting method extracting for noxious material of claim 1 to 4, it is characterized in that, sample is any in pork, pork liver, milk, egg, fruit, vegetables, gastric juice, blood, urine.
6. the QuEChERS extracting method extracting for noxious material is in the application of examination of poisoning by food.
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| CN104569188A (en) * | 2014-12-22 | 2015-04-29 | 青岛康大食品有限公司 | Method for detecting nitrofurazone crude drug |
| CN106872628A (en) * | 2016-11-07 | 2017-06-20 | 上海德诺产品检测有限公司 | A kind of method for determining neoproc content |
| WO2018124862A1 (en) * | 2016-12-30 | 2018-07-05 | École Supérieure Des Industries Du Textile Et De L'habillement (Esith) | Method and extraction kit for determining concentrations of aromatic and aliphatic amines in different matrices |
| CN108680688A (en) * | 2018-05-08 | 2018-10-19 | 江苏安舜技术服务有限公司 | The assay method of BAC and DDAC in a kind of soil and plant-derived product |
| CN109521135A (en) * | 2019-01-18 | 2019-03-26 | 山东省农业科学院农业质量标准与检测技术研究所 | A kind of method that Solid Phase Extraction combination UPLC-MS/MS quickly measures 14 kinds of toxin in Chinese chestnut |
| CN111474279A (en) * | 2020-05-20 | 2020-07-31 | 中国检验检疫科学研究院 | Method and kit for detecting macrolide antibiotic compounds |
| CN111474278A (en) * | 2020-05-20 | 2020-07-31 | 中国检验检疫科学研究院 | Method and kit for detecting metabolites of macrolide compounds |
| CN111595956A (en) * | 2020-04-23 | 2020-08-28 | 浙江大学 | Method for detecting hormone and neurotransmitter in serum |
| CN113155986A (en) * | 2020-12-25 | 2021-07-23 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for detecting perchlorate and chlorate in panax notoginseng |
| CN113340873A (en) * | 2021-08-09 | 2021-09-03 | 北京市疾病预防控制中心 | SERS system for simultaneously detecting multiple toxic substances |
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Cited By (13)
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| CN104569188A (en) * | 2014-12-22 | 2015-04-29 | 青岛康大食品有限公司 | Method for detecting nitrofurazone crude drug |
| CN106872628A (en) * | 2016-11-07 | 2017-06-20 | 上海德诺产品检测有限公司 | A kind of method for determining neoproc content |
| WO2018124862A1 (en) * | 2016-12-30 | 2018-07-05 | École Supérieure Des Industries Du Textile Et De L'habillement (Esith) | Method and extraction kit for determining concentrations of aromatic and aliphatic amines in different matrices |
| CN108680688A (en) * | 2018-05-08 | 2018-10-19 | 江苏安舜技术服务有限公司 | The assay method of BAC and DDAC in a kind of soil and plant-derived product |
| CN109521135B (en) * | 2019-01-18 | 2020-10-23 | 山东省农业科学院农业质量标准与检测技术研究所 | Method for rapidly determining 14 toxins in Chinese chestnut by combining solid phase extraction with UPLC-MS/MS |
| CN109521135A (en) * | 2019-01-18 | 2019-03-26 | 山东省农业科学院农业质量标准与检测技术研究所 | A kind of method that Solid Phase Extraction combination UPLC-MS/MS quickly measures 14 kinds of toxin in Chinese chestnut |
| CN111595956B (en) * | 2020-04-23 | 2021-07-13 | 浙江大学 | Method for detecting hormone and neurotransmitter in serum |
| CN111595956A (en) * | 2020-04-23 | 2020-08-28 | 浙江大学 | Method for detecting hormone and neurotransmitter in serum |
| CN111474278A (en) * | 2020-05-20 | 2020-07-31 | 中国检验检疫科学研究院 | Method and kit for detecting metabolites of macrolide compounds |
| CN111474279A (en) * | 2020-05-20 | 2020-07-31 | 中国检验检疫科学研究院 | Method and kit for detecting macrolide antibiotic compounds |
| CN113155986A (en) * | 2020-12-25 | 2021-07-23 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for detecting perchlorate and chlorate in panax notoginseng |
| CN113155986B (en) * | 2020-12-25 | 2023-01-03 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | Method for detecting perchlorate and chlorate in panax notoginseng |
| CN113340873A (en) * | 2021-08-09 | 2021-09-03 | 北京市疾病预防控制中心 | SERS system for simultaneously detecting multiple toxic substances |
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Application publication date: 20140528 |