CN103698195A - QuEchERS method package for efficiently and homogeneously extracting residues of pesticide and veterinary drug - Google Patents

QuEchERS method package for efficiently and homogeneously extracting residues of pesticide and veterinary drug Download PDF

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Publication number
CN103698195A
CN103698195A CN201310721587.0A CN201310721587A CN103698195A CN 103698195 A CN103698195 A CN 103698195A CN 201310721587 A CN201310721587 A CN 201310721587A CN 103698195 A CN103698195 A CN 103698195A
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bag
veterinary drug
residue
agricultural chemicals
phase
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CN103698195B (en
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郝智清
鹿泽启
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Shandong Qingyun experimental consumables Co., Ltd.
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YANTAI QINGYUN INSTRUMENTS EQUIPMENT Co Ltd
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Abstract

The invention discloses a QuEchERS method package for efficiently and homogeneously extracting residues of a pesticide and a veterinary drug. The QuEchERS method package comprises an extraction pipe containing ammonium sulfate, a buffer salting-out phase-splitting salt package containing a mixture of anhydrous magnesium sulfate and sodium chloride, a needle cylinder type membrane filter containing a mixture of PSA, graphitized carbon black and a C18 reverse phase silica gel filler, and a salting package tool, wherein the PSA is an N-propylethylendiamine-modified silica gel filler and the C18 reverse phase silica gel filler is an octadecyl-modified reverse phase silica gel filler. According to the method, the technical feature of the combination of extraction, salting-out phase-splitting and dehydration purification is fully utilized, devices, materials and operating steps are reasonable to form, the structure is simple, and the operation is easy and convenient.

Description

Efficient homogeneous phase extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug
Technical field
The present invention relates to a kind of method bag of sample pre-treatments, particularly relate to a kind of QuEChERS method bag that extracts agricultural chemicals, residue of veterinary drug for efficient homogeneous phase.
Background technology
QuEChERS is a kind of convenient, efficient Sample Pretreatment Technique detecting for fruits and vegetables class sample Pesticide Residues, the method be take water-miscible organic solvent acetonitrile as extraction agent, by even extraction, the phase-splitting of saltouing, combine with dewatered clean, realized the high efficiency extraction at high-moisture fruits and vegetables sample Pesticide Residues.In order to promote the extensive adaptability of QuEChERS method to several samples and number of chemical character Detecting Pesticide, in Unite States Standard (USS) (AOAC2007.01) and European standard (EN15662), original QuEChERS technology (also claiming original QuEChERS) is improved, to guarantee that the residues of pesticides of pH sensitivity are realized to effectively extraction.In extraction/phase-splitting operation of QuEChERS method, use acetic acid-sodium acetate buffer system or citrate buffer system, adjusting pH is faintly acid, can guarantee that great majority, to acid or alkali labile agricultural chemicals, chemical property change do not occur.
At present, QuEChERS Sample Pretreatment Technique has become the residual detection pre-treatment of fruits and vegetables sample middle peasant standard method in the U.S. and European Union, in China, be also widely applied, but, current method first adds anhydrous magnesium sulfate and inorganic salts in sample extraction process, easily cause magnesium sulfate caking excessive with thermal value, cause volatile residues of pesticides volatilization loss.In addition, in former scheme, the purification of extract adopts in centrifuge tube and adds anhydrous magnesium sulfate and cleanser to be undertaken by centrifuging, and the remaining fine particulate matter in extract can pollute instrument.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of QuEChERS method bag of simple in structure, cost is low, easy and simple to handle, extraction effect is good efficient homogeneous phase extracts agricultural chemicals, residue of veterinary drug.
Efficient homogeneous phase extracts a QuEChERS method bag for agricultural chemicals, residue of veterinary drug, comprising:
Extracting tube, its inside comprises ammonium sulfate;
Cushion the phase-splitting salt bag of saltouing, its inside comprises the potpourri of anhydrous magnesium sulfate and sodium chloride;
Syringe-type membrane filter, its inside comprises the potpourri of PSA, ketjenblack EC and C18 reverse phase silica gel filler;
Salt adding job contract tool;
Wherein, described PSA is the ethylene diamine-modified silica filler of N-propyl group, and described C18 reverse phase silica gel filler is the reverse phase silica gel filler that octadecyl is modified.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, and the specification of wherein said extracting tube is 15ml or 50ml, and its inside comprises the ammonium sulfate of 100mg.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, the wherein said buffering potpourri that phase-splitting salt bag inside comprises that the anhydrous magnesium sulfate of 2-4g and the sodium chloride of 0.5-1.5g mix of saltouing.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, and wherein said syringe-type membrane filter inside comprises the potpourri that the C18 reverse phase silica gel filler of the PSA of 25mg, the ketjenblack EC of 25mg and 25mg mixes.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, and wherein said salt adding job contract tool is that length and width specification is the white light facial tissue of 70mm*70mm.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, the wherein said buffering square salt bag that phase-splitting salt bag is 70mm*70mm for the length and width specification made by aluminium foil and polyethylene composite film of saltouing.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, and wherein said extracting tube and described syringe-type membrane filter are made by PE material.
Efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, also comprise for holding the saltout bag of phase-splitting salt bag, syringe-type membrane filter and described salt adding job contract tool of described extracting tube, described buffering, described bag is made by foil laminated film, and length and width are 200mm*150mm.
The QuEChERS method bag that adopts efficient homogeneous phase of the present invention to extract agricultural chemicals, residue of veterinary drug carries out a method for sample pre-treatments, comprises the steps:
Step 1, get 5g sample in extracting tube, and add 5ml acetonitrile in described extracting tube, vortex concussion 1-2 minute, the efficient homogeneous phase extraction of medicine;
Step 2, the material that uses salt adding job contract tool that buffering is saltoutd in phase-splitting salt bag add the phase-splitting of dewatering in described extracting tube, vortex concussion centrifugal 1-2 minute after 1-2 minute;
Step 3, the supernatant 1ml getting in described extracting tube are placed in syringe-type membrane filter, vortex vibration 1-2 minute, and the sample after purification is released by described syringe-type membrane filter, is directly used in instrumental analysis.
The method of sample pre-treatments of the present invention, wherein said sample is fruits and vegetables, meat, aquatic products, grain, drinks, tealeaves or tobacco.
The QuEChERS method bag difference from prior art that efficient homogeneous phase of the present invention extracts agricultural chemicals, residue of veterinary drug is:
The ultimate principle of the QuEChERS method bag of efficient homogeneous phase extraction agricultural chemicals of the present invention, residue of veterinary drug based on QuEChERS, the technical characterstic that make full use of extraction, the phase-splitting of saltouing combines with dewatered clean, device, material and operation steps form rationally, have overcome defect of the prior art.
The present invention is in QuEChERS method frame, propose first to add a small amount of ammonium sulfate and acetonitrile to carry out homogeneous phase extraction in sample, be used in conjunction with so the efficient homogeneous phase extraction that can realize residues of pesticides, add again anhydrous magnesium sulfate and sodium chloride to play the effect of buffering, dehydration, phase-splitting, to realize efficient minute phase dehydration, simultaneously, the present invention realizes the purification of extract with syringe filtering type clarifier, this filter bottom is equipped with filtering membrane, after vortex vibration, then, directly by push rod, sample is pushed to sample bottle for Instrument measuring.
The QuEChERS method bag tool that efficient homogeneous phase of the present invention extracts agricultural chemicals, residue of veterinary drug has the following advantages:
(1) use the ammonium sulfate in acetonitrile and the method for the invention bag to extract, replaced original acetonitrile solution scheme that adds 1% acetic acid, the pH value that ammonium sulfate can guarantee solution with add the acetic acid-sodium acetate buffer system result in former method the same, but more convenient operation, the present invention directly adds ammonium sulfate in extracting tube, and user of service only need add a kind of conventional solution of acetonitrile;
(2) be equipped with special-purpose salt adding job contract tool, be convenient to Jiang Yanbao and add in extracting tube, while avoiding directly being imported by sack, spill, and convenient and swift;
(3) adopt syringe-type membrane filter purification style, do not adopt traditional centrifuge tube Depurative design, without centrifugal, only need vortex vibration or hand, can loading analysis.
The method of the invention bag application is wide, be applicable to all laboratories that need to use QuEChERS method to carry out residues of pesticides, residue of veterinary drug analysis, comprise the laboratory in the industries such as vegetables, fruit, grain, aquatic products, meat of poultris, meat, tealeaves, tobacco, drinks; Adopt the method for the invention bag for needing to add water such as the moisture less or dryness sample such as animal food, cereal, dry fruit, tobacco or tealeaves to weaken interaction between agricultural chemicals and matrix to guarantee abundant phase-splitting before extraction, even high fat content sample, as avocado or olive oils plant, also can be analyzed by the method for the invention bag.
The QuEChERS method bag that efficient homogeneous phase of the present invention is extracted to agricultural chemicals, residue of veterinary drug below in conjunction with accompanying drawing is described further.
Accompanying drawing explanation
Fig. 1 is the structural representation that efficient homogeneous phase of the present invention extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug.
Embodiment
Embodiment 1
As shown in Figure 1, the QuEChERS method bag of the efficient homogeneous phase extraction of the present invention agricultural chemicals, residue of veterinary drug comprises:
Extracting tube 1, its inside comprises ammonium sulfate; Cushion the phase-splitting salt bag 2 of saltouing, its inside comprises the potpourri of anhydrous magnesium sulfate and sodium chloride; Syringe-type membrane filter 3, its inside comprises the potpourri of PSA, ketjenblack EC and C18 reverse phase silica gel filler; Salt adding job contract tool 4; Wherein, described PSA is the ethylene diamine-modified silica filler of N-propyl group, and described C18 reverse phase silica gel filler is the reverse phase silica gel filler that octadecyl is modified.
Embodiment 2
As shown in Figure 1, the QuEChERS method bag of the efficient homogeneous phase extraction of the present invention agricultural chemicals, residue of veterinary drug comprises:
Extracting tube 1, its inside comprises ammonium sulfate; Cushion the phase-splitting salt bag 2 of saltouing, its inside comprises the potpourri of anhydrous magnesium sulfate and sodium chloride; Syringe-type membrane filter 3, its inside comprises the potpourri of PSA, ketjenblack EC and C18 reverse phase silica gel filler; Salt adding job contract tool 4; Wherein, described PSA is the ethylene diamine-modified silica filler of N-propyl group, and described C18 reverse phase silica gel filler is the reverse phase silica gel filler that octadecyl is modified.
The specification of described extracting tube 1 is 15ml, and its inside comprises the ammonium sulfate of 100mg; Described buffering phase-splitting salt bag 2 inside of saltouing comprise the potpourri that the anhydrous magnesium sulfate of 2g and the sodium chloride of 1.5g mix; Described syringe-type membrane filter 3 inside comprise the potpourri that the C18 reverse phase silica gel filler of the PSA of 25mg, the ketjenblack EC of 25mg and 25mg mixes; The white light facial tissue that described salt adding job contract tool 4 is 70mm*70mm for length and width specification.The described buffering square salt bag that phase-splitting salt bag 2 is 70mm*70mm for the length and width specification made by aluminium foil and polyethylene composite film of saltouing; Described extracting tube 1 and described syringe-type membrane filter 3 are made by PE material.
The QuEChERS method bag that efficient homogeneous phase of the present invention extracts agricultural chemicals, residue of veterinary drug also comprises for holding the saltout bag 5 of phase-splitting salt bag 2, syringe-type membrane filter 3 and described salt adding job contract tool 4 of described extracting tube 1, described buffering, described bag 5 is made by foil laminated film, and length and width are 200mm*150mm.
Embodiment 3
Be with the difference of embodiment 2: the specification of described extracting tube 1 is 50ml, described buffering phase-splitting salt bag 2 inside of saltouing comprise the potpourri that the anhydrous magnesium sulfate of 4g and the sodium chloride of 0.5g mix.
Embodiment 4
Be with the difference of embodiment 2: the specification of described extracting tube 1 is 15ml, described buffering phase-splitting salt bag 2 inside of saltouing comprise the potpourri that the anhydrous magnesium sulfate of 3g and the sodium chloride of 1g mix.
Embodiment 5
The QuEChERS method bag that adopts efficient homogeneous phase of the present invention to extract agricultural chemicals, residue of veterinary drug carries out a method for sample pre-treatments, it is characterized in that: comprise the steps:
Step 1, get 5g sample in extracting tube 1, and in described extracting tube 1, add 5ml acetonitrile, vortex concussion 1-2 minute, the efficient homogeneous phase extraction of medicine;
Step 2, the material that uses salt adding job contract tool 4 that buffering is saltoutd in phase-splitting salt bag 2 add the phase-splitting of dewatering in described extracting tube 1, vortex concussion centrifugal 1-2 minute after 1-2 minute;
Step 3, the supernatant 1ml getting in described extracting tube 1 are placed in syringe-type membrane filter 3, vortex vibration 1-2 minute, and the sample after purification is released by described syringe-type membrane filter 3, is directly used in instrumental analysis.
Wherein, described sample is fruits and vegetables, meat, aquatic products, grain, drinks, tealeaves or tobacco.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.

Claims (10)

1. efficient homogeneous phase extracts a QuEChERS method bag for agricultural chemicals, residue of veterinary drug, it is characterized in that: comprising:
Extracting tube (1), its inside comprises ammonium sulfate;
Cushion the phase-splitting salt bag (2) of saltouing, its inside comprises the potpourri of anhydrous magnesium sulfate and sodium chloride;
Syringe-type membrane filter (3), its inside comprises the potpourri of PSA, ketjenblack EC and C18 reverse phase silica gel filler;
Salt adding job contract tool (4);
Wherein, described PSA is the ethylene diamine-modified silica filler of N-propyl group, and described C18 reverse phase silica gel filler is the reverse phase silica gel filler that octadecyl is modified.
2. efficient homogeneous phase according to claim 1 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: the specification of described extracting tube (1) is 15ml or 50ml, and its inside comprises the ammonium sulfate of 100mg.
3. efficient homogeneous phase according to claim 1 and 2 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: described buffering phase-splitting salt bag (2) inside of saltouing comprises the potpourri that the anhydrous magnesium sulfate of 2-4g and the sodium chloride of 0.5-1.5g mix.
4. efficient homogeneous phase according to claim 3 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: described syringe-type membrane filter (3) inside comprises the potpourri that the C18 reverse phase silica gel filler of the PSA of 25mg, the ketjenblack EC of 25mg and 25mg mixes.
5. efficient homogeneous phase according to claim 4 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: the white light facial tissue that described salt adding job contract tool (4) is 70mm*70mm for length and width specification.
6. efficient homogeneous phase according to claim 3 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: the described buffering square salt bag that phase-splitting salt bag (2) is 70mm*70mm for the length and width specification made by aluminium foil and polyethylene composite film of saltouing.
7. efficient homogeneous phase according to claim 1 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: described extracting tube (1) and described syringe-type membrane filter (3) are made by PE material.
8. efficient homogeneous phase according to claim 1 extracts the QuEChERS method bag of agricultural chemicals, residue of veterinary drug, it is characterized in that: also comprise for holding the saltout bag (5) of phase-splitting salt bag (2), syringe-type membrane filter (3) and described salt adding job contract tool (4) of described extracting tube (1), described buffering, described bag (5) is made by foil laminated film, and length and width are 200mm*150mm.
9. the QuEChERS method bag that adopts in claim 1-8 efficient homogeneous phase described in any one to extract agricultural chemicals, residue of veterinary drug carries out a method for sample pre-treatments, it is characterized in that: comprise the steps:
Step 1, get 5g sample in extracting tube (1), and add 5ml acetonitrile in described extracting tube (1), vortex concussion 1-2 minute, the efficient homogeneous phase extraction of medicine;
Step 2, the material that uses salt adding job contract tool (4) that buffering is saltoutd in phase-splitting salt bag (2) add the phase-splitting of dewatering in described extracting tube (1), vortex concussion centrifugal 1-2 minute after 1-2 minute;
Step 3, the supernatant 1ml getting in described extracting tube (1) are placed in syringe-type membrane filter (3), vortex vibration 1-2 minute, and the sample after purification is released by described syringe-type membrane filter (3), is directly used in instrumental analysis.
10. the method for sample pre-treatments according to claim 9, is characterized in that: described sample is fruits and vegetables, meat, aquatic products, grain, drinks, tealeaves or tobacco.
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Cited By (14)

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TWI500915B (en) * 2014-07-18 2015-09-21 Agricultural Chemicals And Toxic Substances Res Inst Council Of Agriculture A quick extraction kit for a procedure of detecting pesticide residues in agricultural products and a method of taking primary test liquid from agricultural sample by the quick extraction kit
CN105021717A (en) * 2014-04-29 2015-11-04 中国水产科学研究院 Method for measuring residual quantity of ethyl 3-aminobenzoate in aquatic product
CN105092352A (en) * 2015-07-17 2015-11-25 郭礼强 Recovery utilization method for mycotoxin QuEChERS purifying powder
CN105092353A (en) * 2015-07-17 2015-11-25 丁葵英 Recovery utilization method for pesticide residue QuEChERS purifying powder
CN106770786A (en) * 2017-01-11 2017-05-31 重庆市农业科学院 A kind of garden stuff pesticide residue detects fast purification device
CN106770841A (en) * 2017-03-23 2017-05-31 西北师范大学 The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques
CN107576744A (en) * 2017-09-29 2018-01-12 沈阳出入境检验检疫局检验检疫综合技术中心 A kind of method for detecting animal derived food veterinary drug residue
CN107831053A (en) * 2017-08-29 2018-03-23 暨南大学 It is a kind of rapidly and efficiently to extract the methods and applications of antibiotic and its metabolin in plant sample
CN107976490A (en) * 2017-09-29 2018-05-01 沈阳出入境检验检疫局检验检疫综合技术中心 The remaining method of pesticide in one kind detection veterinary antibiotics
CN108593824A (en) * 2018-06-08 2018-09-28 中国水稻研究所 A kind of pre-treatment purification method of gas chromatography mass spectrometry Detecting Pesticide
CN109001312A (en) * 2018-07-04 2018-12-14 上海德易检测技术有限公司 A kind of detection method of pesticide residues in fruits
CN111713465A (en) * 2020-07-10 2020-09-29 张俊中 Aquatic product quality detection and capture device and implementation method thereof
WO2020220618A1 (en) * 2019-04-30 2020-11-05 华南理工大学 One-step quechers pretreatment device
CN113533590A (en) * 2020-04-14 2021-10-22 内蒙古伊利实业集团股份有限公司 Pretreatment method for detecting pesticide residue in milk, dairy products and grain powder

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Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105021717A (en) * 2014-04-29 2015-11-04 中国水产科学研究院 Method for measuring residual quantity of ethyl 3-aminobenzoate in aquatic product
TWI500915B (en) * 2014-07-18 2015-09-21 Agricultural Chemicals And Toxic Substances Res Inst Council Of Agriculture A quick extraction kit for a procedure of detecting pesticide residues in agricultural products and a method of taking primary test liquid from agricultural sample by the quick extraction kit
CN105092352A (en) * 2015-07-17 2015-11-25 郭礼强 Recovery utilization method for mycotoxin QuEChERS purifying powder
CN105092353A (en) * 2015-07-17 2015-11-25 丁葵英 Recovery utilization method for pesticide residue QuEChERS purifying powder
CN105092352B (en) * 2015-07-17 2017-09-26 郭礼强 A kind of recoverying and utilizing method of mycotoxin QuEChERS purified powders
CN105092353B (en) * 2015-07-17 2017-10-03 丁葵英 A kind of recoverying and utilizing method of residues of pesticides QuEChERS purified powders
CN106770786A (en) * 2017-01-11 2017-05-31 重庆市农业科学院 A kind of garden stuff pesticide residue detects fast purification device
CN106770841A (en) * 2017-03-23 2017-05-31 西北师范大学 The method that fruit Pesticides Testing sample is processed using QuEChERS abstraction techniques
CN107831053B (en) * 2017-08-29 2020-12-22 暨南大学 Method for rapidly and efficiently extracting antibiotics and metabolites thereof from plant sample and application
CN107831053A (en) * 2017-08-29 2018-03-23 暨南大学 It is a kind of rapidly and efficiently to extract the methods and applications of antibiotic and its metabolin in plant sample
CN107576744A (en) * 2017-09-29 2018-01-12 沈阳出入境检验检疫局检验检疫综合技术中心 A kind of method for detecting animal derived food veterinary drug residue
CN107976490A (en) * 2017-09-29 2018-05-01 沈阳出入境检验检疫局检验检疫综合技术中心 The remaining method of pesticide in one kind detection veterinary antibiotics
CN108593824A (en) * 2018-06-08 2018-09-28 中国水稻研究所 A kind of pre-treatment purification method of gas chromatography mass spectrometry Detecting Pesticide
CN109001312A (en) * 2018-07-04 2018-12-14 上海德易检测技术有限公司 A kind of detection method of pesticide residues in fruits
WO2020220618A1 (en) * 2019-04-30 2020-11-05 华南理工大学 One-step quechers pretreatment device
CN113533590A (en) * 2020-04-14 2021-10-22 内蒙古伊利实业集团股份有限公司 Pretreatment method for detecting pesticide residue in milk, dairy products and grain powder
CN111713465A (en) * 2020-07-10 2020-09-29 张俊中 Aquatic product quality detection and capture device and implementation method thereof

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Address after: 264000 Airport Road, Zhifu, Shandong, No. 80, No.

Patentee after: Shandong Qingyun experimental consumables Co., Ltd.

Address before: 264000 Laishan science and technology, Shandong Province, the main street, science and technology building, room B, room 508,

Patentee before: YANTAI QINGYUN INSTRUMENTS EQUIPMENT CO., LTD.