CN104359844A - Detection method for pesticide residues of vegetables and fruits - Google Patents
Detection method for pesticide residues of vegetables and fruits Download PDFInfo
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- CN104359844A CN104359844A CN201410653960.8A CN201410653960A CN104359844A CN 104359844 A CN104359844 A CN 104359844A CN 201410653960 A CN201410653960 A CN 201410653960A CN 104359844 A CN104359844 A CN 104359844A
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Abstract
The invention relates to a detection method for pesticide residues of vegetables and fruits. The method comprises the following steps: A, cutting a to-be-detected sample after washing by using clean water into 3*3mm bulky fragments; B, putting 5g of the fragments in a centrifuge tube, adding 10ml of distilled water or a buffer solution at 30-40 DEG C, shaking for about 50 times and standing for 2-5 minutes; C, adding 5-10g of a solvent and putting the centrifuge tube in an oscillator for extraction for 3 minutes, and transferring an extraction liquid to another centrifuge tube; D, adding 2-5g of a purifier, shaking for 5 minutes, standing for 5 minutes, absorbing upper solution, directly connecting to a needle-cylinder filter, filtering suspended solids in the solution, and collecting the filtrate in a test tube; E, putting the test tube filled with the filtrate in a water bath at 30 DEG C and thoroughly blowing the solvent in the test tube by air; and F, measuring orthophosphate by classical phosphomolybdenum blue spectrophotometric method and calculating the total residues of organophosphorus pesticide in the vegetable sample according to the measured orthophosphate concentration. The method is mature and reliable in principle, simple and convenient to operate, low in price of instruments, low in measuring cost and high in measuring accuracy and sensitivity.
Description
Technical field
The present invention relates to a kind of method of detection of veterinary antibiotics Pesticide Residues, belong to vegetable pesticide residue detection field.
Background technology
The agricultural chemicals that China commonly uses at present, can be divided into organophosphorus, organochlorine (chrysanthemum ester class, benzene hexachloride, DDT, chloromycetin) and organic nitrogen (carbamates, sulfamido) three major types.Literature query result shows, the method measuring Organophosphorus and carbamate pesticides residues of pesticides in vegetables at present both at home and abroad mainly contains chromatography, inhibiting AChE, speed survey clever method, polarography, biphenylamine development process, euzymelinked immunosorbent assay (ELISA) etc.Wherein chromatography, inhibiting AChE, speed are surveyed clever method and are obtained practical application.Domestic similar research concentrates on chromatography and inhibiting AChE.Both detection method standardization all, becomes the examination criteria of country and industry.Inhibiting AChE generally uses fast detection method at present.But measurement result is not accurate enough, false positive and false negative result happen occasionally, and testing cost is also higher.Chromatographic testing result is accurate, but length consuming time, testing cost is high.The invention provides one and can be used for the units such as Vegetable produce base, wholesale market of agricultural products and epidemic prevention department, fast and accurately measure the low cost of Organo-phosphorus Pesticide Residues in Vegetables amount, high-sensitive technology.Little to the sensitivity difference of different agricultural chemicals, thus can set residues of pesticides more scientificly and to exceed standard limit value; The half-quantitative detection to organophosphorus pesticide can be realized.
Summary of the invention
The object of the present invention is to provide a kind of method of detection of veterinary antibiotics Pesticide Residues, mainly solve the problem existing for above-mentioned prior art, whether can be detected fast in veterinary antibiotics, melon beans containing organophosphorus insecticide by said method, its principle mature and reliable, easy and simple to handle, instrument price is cheap, testing cost is low, accuracy of measurement and highly sensitive, has very strong competitive power.
For achieving the above object, technical scheme of the present invention is:
A method for the detection of veterinary antibiotics Pesticide Residues, is characterized in that: its operation steps is:
A is cut into the block fragment of 3 × 3mm after being rinsed sample clear water to be detected;
B gets 5g fragment and puts into centrifuge tube, adds 10ml, the distilled water of 30 DEG C ~ 40 DEG C or buffer solution, jolts about 50 times, leaves standstill 2 ~ 5 minutes;
C adds a kind of 5 ~ 10g solvent and centrifuge tube is placed in oscillator and extracts 3min, is transferred to by extract in another centrifuge tube;
D adds a kind of 2 ~ 5g cleanser, and vibration 5min, draws upper solution after leaving standstill 5 min, and directly access syringe filter disk, and filter the suspension removed in solution, filtrate is collected in test tube;
The test tube that filtrate is housed is placed in the water-bath that temperature is 30 DEG C by E, is purged by the solvent in test tube clean with air;
F, with the P-Mo blue spectrophotometry orthophosphate of classics, calculates the total residue of organophosphorus pesticide in vegetable sample by the orthophosphate densimeter measured.
The method of the detection of described veterinary antibiotics Pesticide Residues, is characterized in that: the solvent of described step C is the wherein one of non-ionic surfactant three oleic acid sorb ester, hydroxy stearic acid hydroxyl octacosane ester.
The method of the detection of described veterinary antibiotics Pesticide Residues, is characterized in that: in described step D, cleanser is the wherein one of potassium persulfate, ammonium persulfate.
The advantage that formula of the present invention and method can embody is:
Whether the method for the detection of the veterinary antibiotics Pesticide Residues announced by the present invention can be detected in veterinary antibiotics, melon beans fast containing organophosphorus insecticide, its principle mature and reliable, easy and simple to handle, instrument price is cheap, testing cost is low, accuracy of measurement and highly sensitive, has very strong competitive power.
Embodiment
Embodiment 1: a kind of method of detection of veterinary antibiotics Pesticide Residues.It comprises the steps:
1, the block fragment of 3 × 3mm is cut into after being rinsed sample Xiaoqinling Nature Reserve 20g clear water to be detected;
2, get 5g fragment and put into centrifuge tube, add 10ml, the distilled water of 35 DEG C or buffer solution, jolt about 50 times, leave standstill 2 ~ 5 minutes;
3, add 10g tri-oleic acid sorb ester and centrifuge tube is placed in oscillator and extract 3min, extract is transferred in another centrifuge tube;
4, add 2g potassium persulfate, vibration 5min, draws upper solution after leaving standstill 5 min, and directly accesses syringe filter disk, and filter the suspension removed in solution, filtrate is collected in test tube;
5, the test tube that filtrate is housed is placed in the water-bath that temperature is 30 DEG C, the solvent in test tube is purged clean with air;
6, with the P-Mo blue spectrophotometry orthophosphate of classics, the total residue being calculated organophosphorus pesticide in vegetable sample by the orthophosphate densimeter measured is 0.13mg/kg.
Embodiment 2: a kind of method of detection of veterinary antibiotics Pesticide Residues.It comprises the steps:
1, the block fragment of 3 × 3mm is cut into after being rinsed sample apple 20g clear water to be detected;
2, get 5g fragment and put into centrifuge tube, add 10ml, the distilled water of 35 DEG C or buffer solution, jolt about 50 times, leave standstill 2 ~ 5 minutes;
3, add 10g hydroxy stearic acid hydroxyl octacosane ester and centrifuge tube is placed in oscillator and extract 3min, extract is transferred in another centrifuge tube;
4, add 10g ammonium persulfate, vibration 5min, draws upper solution after leaving standstill 5 min, and directly accesses syringe filter disk, and filter the suspension removed in solution, filtrate is collected in test tube;
5, the test tube that filtrate is housed is placed in the water-bath that temperature is 30 DEG C, the solvent in test tube is purged clean with air;
6, with the P-Mo blue spectrophotometry orthophosphate of classics, the total residue being calculated organophosphorus pesticide in vegetable sample by the orthophosphate densimeter measured is 0.15mg/kg.
Be only preferred embodiment of the present invention in sum, be not used for limiting practical range of the present invention.Namely all equivalences done according to the content of the present patent application the scope of the claims change and modify, and all should be technology category of the present invention.
Claims (3)
1. a method for the detection of veterinary antibiotics Pesticide Residues, is characterized in that: its operation steps is:
A is cut into the block fragment of 3 × 3mm after being rinsed sample clear water to be detected;
B gets 5g fragment and puts into centrifuge tube, adds 10ml, the distilled water of 30 DEG C ~ 40 DEG C or buffer solution, jolts about 50 times, leaves standstill 2 ~ 5 minutes;
C adds a kind of 5 ~ 10g solvent and centrifuge tube is placed in oscillator and extracts 3min, is transferred to by extract in another centrifuge tube;
D adds a kind of 2 ~ 5g cleanser, and vibration 5min, draws upper solution after leaving standstill 5 min, and directly access syringe filter disk, and filter the suspension removed in solution, filtrate is collected in test tube;
The test tube that filtrate is housed is placed in the water-bath that temperature is 30 DEG C by E, is purged by the solvent in test tube clean with air;
F, with the P-Mo blue spectrophotometry orthophosphate of classics, calculates the total residue of organophosphorus pesticide in vegetable sample by the orthophosphate densimeter measured.
2. the method for the detection of veterinary antibiotics Pesticide Residues according to claim 1, is characterized in that: the solvent of described step C is the wherein one of non-ionic surfactant three oleic acid sorb ester, hydroxy stearic acid hydroxyl octacosane ester.
3. the method for the detection of veterinary antibiotics Pesticide Residues according to claim 1 and 2, is characterized in that: in described step D, cleanser is the wherein one of potassium persulfate, ammonium persulfate.
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CN201410653960.8A CN104359844A (en) | 2014-11-18 | 2014-11-18 | Detection method for pesticide residues of vegetables and fruits |
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CN201410653960.8A CN104359844A (en) | 2014-11-18 | 2014-11-18 | Detection method for pesticide residues of vegetables and fruits |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105241988A (en) * | 2015-09-23 | 2016-01-13 | 广西南宁民安检测技术有限公司 | Method used for detecting fruit pesticide residue |
CN106323896A (en) * | 2016-11-09 | 2017-01-11 | 无锡艾科瑞思产品设计与研究有限公司 | Detection method of carbofuran residues |
CN107300530A (en) * | 2017-06-28 | 2017-10-27 | 防城港市质量技术监督局 | The detection method of fruit residues of pesticides |
CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
CN110346342A (en) * | 2019-08-28 | 2019-10-18 | 苏银华 | A kind of pesticide residue detection method |
CN112378904A (en) * | 2020-11-24 | 2021-02-19 | 临沂华澳食品有限公司 | Rapid detection method for pesticide residues in melons, fruits and vegetables |
-
2014
- 2014-11-18 CN CN201410653960.8A patent/CN104359844A/en active Pending
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105241988A (en) * | 2015-09-23 | 2016-01-13 | 广西南宁民安检测技术有限公司 | Method used for detecting fruit pesticide residue |
CN106323896A (en) * | 2016-11-09 | 2017-01-11 | 无锡艾科瑞思产品设计与研究有限公司 | Detection method of carbofuran residues |
CN107300530A (en) * | 2017-06-28 | 2017-10-27 | 防城港市质量技术监督局 | The detection method of fruit residues of pesticides |
CN107389808A (en) * | 2017-06-28 | 2017-11-24 | 防城港市质量技术监督局 | The detection method of vegetable pesticide residue |
CN110346342A (en) * | 2019-08-28 | 2019-10-18 | 苏银华 | A kind of pesticide residue detection method |
CN110346342B (en) * | 2019-08-28 | 2021-12-21 | 苏银华 | Pesticide residue detection method |
CN112378904A (en) * | 2020-11-24 | 2021-02-19 | 临沂华澳食品有限公司 | Rapid detection method for pesticide residues in melons, fruits and vegetables |
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Application publication date: 20150218 |