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.
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.