CN102967673A - Method for detecting difference of residual chlorpyrifos in rapes washed in different ways - Google Patents
Method for detecting difference of residual chlorpyrifos in rapes washed in different ways Download PDFInfo
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- CN102967673A CN102967673A CN2012105009484A CN201210500948A CN102967673A CN 102967673 A CN102967673 A CN 102967673A CN 2012105009484 A CN2012105009484 A CN 2012105009484A CN 201210500948 A CN201210500948 A CN 201210500948A CN 102967673 A CN102967673 A CN 102967673A
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Abstract
The invention discloses a method for detecting the difference of residual chlorpyrifos in rapes washed in different ways. The method comprises the steps of after harvesting the rapes treated by using the chlorpyrifos, randomly selecting rape plants and taking leaves of the rape plants as samples; and selecting different washing ways to wash the samples, preparing the samples into sample solutions after the washing, respectively carrying out gas chromatography on the sample solutions and a reference sample solution through using a gas chromatographic method so as to obtain the difference of the chlorpyrifos content through calculating and comparing a spectral peak area. By means of the method, the situation of the change of the chlorpyrifos residual amount level in the rapes washed in the different ways can be clearly and conveniently obtained through adopting the gas chromatographic method, so that the condition that which washing way can more effectively reduce the residual chlorpyrifos in the rapes is confirmed and the guidance in vegetable safety eating aspect can be provided for people in daily life.
Description
Technical field
The present invention relates to a kind of detection method of different modes being cleaned the difference of residual chlopyrifos in the rear rape.
Background technology
Countries in the world all exist the different Pesticide Residue of degree, raising along with people's living standard, people more and more pay attention to food-safety problem, food safety and sanitation not only is related to human health, survival and development, also is the problem that national governments and WHO show great attention to and pay attention to simultaneously.Rape is one of requisite food in people's diet, and the necessary multivitamin of human body and mineral matter can be provided.Also contain diversified plant biological active substance in the rape, be people generally acknowledge to the effective composition of health.But in present agricultural production, vegetables are that agricultural chemicals is relied on one of larger crops.In order to guarantee the high yield good harvest of vegetables, a large amount of agricultural chemicals are used even abuse.Need the continuous several times applying pesticides before the ripe listing of overwhelming majority vegetables, cause the vegetable pesticide residue severe overweight, not only to environment, and health caused in various degree infringement.Although various places have been formulated many kinds of measures and have been maintained strict control over the vegetable safety pass, forbid exceed standard vegetables listing of residues of pesticides, a lot of vegetable pesticide residue events of exceeding standard are had a lingering fear the rank and file when edible vegetable.At present, therefore the consumer, is necessary to analyze under different mode of washing owing to excessively panic to the vegetable safety problem, and whether pesticide residue has variation to a certain degree.Can be people's daily life provides the guidance of the edible aspect of vegetable safety.
Chlopyrifos is the organophosphorus pesticide kind of the unique license of the World Health Organization (WHO), also is one of insecticide variety of present produced worldwide and sales volume maximum.Chlopyrifos is a kind of broad spectrum insecticide, this kind have tag, stomach toxicity and stifling three kinds of modes of action, eyes are had slight stimulation, skin is had obvious stimulation, Long contact time can skin ambustion.Under test dose, have no teratogenesis, mutagenesis, carcinogenesis.According to national standard, the leaf vegetables that all chlorpyrifos pesticide residue quantitative measurements are lower than 0.1mg/kg all meets national standard, does not consist of health and threatens.Residual chlopyrifos difference detects in the rear rape and also can't clean different modes at present, thereby it is lower to determine which kind of cleaning way can guarantee to clean chlopyrifos residual in the rear rape.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of detection method of different modes being cleaned the difference of residual chlopyrifos in the rear rape, can determine the difference of residual chlopyrifos in the rape after different modes cleans, thereby solve after detecting at present different modes and cleaning the difference of residual chlopyrifos in the rape, can not determine which kind of cleaning way can guarantee to clean the lower problem of chlopyrifos residual in the rear rape.
Above-mentioned technical matters can solve by the following technical programs:
The embodiment of the invention provides a kind of detection method to the difference of residual chlopyrifos in the rape after the different modes cleaning, comprising:
After will gathering with the rape that chlopyrifos is processed, randomly draw rapeseed plants, get the blade of described rapeseed plants as sample;
Choosing different cleaning ways cleans described sample, after the cleaning described sample is made sample solution, described sample solution is carried out gas chromatographic analysis with reference substance solution by vapor-phase chromatography respectively, draw the difference of chlopyrifos content by calculating the spectrum peak area ratio.
Method of the present invention, the sample solution of the rear rape leaf of different modes cleaning being made by vapor-phase chromatography detects, can compare the difference that different modes cleans residual chlopyrifos in the rear rape by calculating the spectrum peak area, thereby determine which kind of cleaning way can more effective removal rape in residual chlopyrifos, have simple, the easy advantage of row.
Description of drawings
In order to be illustrated more clearly in the technical scheme of the embodiment of the invention, the accompanying drawing of required use was done to introduce simply during the below will describe embodiment, apparently, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite of not paying creative work, can also obtain other accompanying drawings according to these accompanying drawings.
The comparison diagram of the rape Chlorpyrifos Residue difference behind six durations of clear water soaking and washing that the method that Fig. 1 provides for the embodiment of the invention detects;
The comparison diagram of the rape Chlorpyrifos Residue difference behind six durations of detersive soaking and washing that the method that Fig. 2 provides for the embodiment of the invention detects;
The saline sook that the method that Fig. 3 provides for the embodiment of the invention detects cleans the comparison diagram of the rape Chlorpyrifos Residue difference behind six durations;
The comparison diagram of the rape Chlorpyrifos Residue difference behind six durations of rice washing water soaking and washing that the method that Fig. 4 provides for the embodiment of the invention detects;
Each cleaning way that the method that Fig. 5 provides for the embodiment of the invention detects soaks the comparison diagram of 5 minutes rape Chlorpyrifos Residue amount;
Each cleaning way that the method that Fig. 6 provides for the embodiment of the invention detects soaks the comparison diagram of 15 minutes rape Chlorpyrifos Residue amount.
Embodiment
The below is clearly and completely described the technical scheme in the embodiment of the invention, and obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on embodiments of the invention, those of ordinary skills belong to protection scope of the present invention not making the every other embodiment that obtains under the creative work prerequisite.
The embodiment of the invention provides a kind of detection method to the difference of residual chlopyrifos in the rape after the different modes cleaning, may further comprise the steps:
After will gathering with the rape that chlopyrifos is processed, randomly draw rapeseed plants, get the blade of described rapeseed plants as sample;
Choosing different cleaning ways cleans described sample, after the cleaning sample is made sample solution, sample solution is carried out gas chromatographic analysis with reference substance solution by vapor-phase chromatography respectively, draw the difference of chlopyrifos content by calculating the spectrum peak area ratio.
In the said method, different cleaning ways comprise: clear water soaking and washing, saline sook cleaning, rice washing water soaking and washing or detersive soaking and washing.The soak time of each soaking and washing mode is respectively: 5 minutes, 15 minutes, 30 minutes, 60 minutes, 120 minutes.
In the said method, described sample after will cleaning is in the following manner made sample solution, comprise: the described sample after will cleaning shreds and is placed in the mortar, after fully grinding, take by weighing the 5g stamping in centrifuge tube, add the 15mL hexane extract, place in the supersonic wave cleaning machine ultrasonic extraction after 15 minutes, in hydro-extractor with 3000rmin
-1Centrifugal 8 minutes of rotating speed; Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters round-bottomed flask, washs the glass funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the round-bottomed flask; With Rotary Evaporators the solution in the described round-bottomed flask is condensed into the 2mL concentrate, described concentrate is settled to 5mL with normal hexane, namely gets sample solution.
In the said method, reference substance solution makes in the following manner, comprising:
Rape leaf shredded be placed in the mortar, after fully grinding, take by weighing the 5g stamping in centrifuge tube, add the 15mL hexane extract, place in the supersonic wave cleaning machine ultrasonic extraction after 15 minutes, in hydro-extractor with 3000rmin
-1Centrifugal 8 minutes of rotating speed; Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters round-bottomed flask, washs the funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the described round-bottomed flask; With Rotary Evaporators the solution in the described round-bottomed flask is condensed into the 2mL concentrate, described concentrate is settled to 5mL with normal hexane, namely gets reference substance solution.
In the said method, adopt fresh blade as the blade of the rapeseed plants of sample, can adopt plucking time to be no more than the blade of 1 hour rapeseed plants.
Below in conjunction with specific embodiment said method is described further.
Concrete steps are: experimental cultivar breeding cultivation → sprinkling chlopyrifos → extraction test sample → the carry out processing → reference substance of different washing agent and different soak times and the preparation of test solution → carry out gas chromatography → data analysis
(1) breeding cultivation of experimental cultivar:
Select the rape variety of common high-quality, in the little shed in land, experimental center in 2010, plant;
(2) spray chlopyrifos:
Spray chlopyrifos in January, 2011, evenly be sprayed at watering can on the blade of rape, spray chlopyrifos and preferably be selected in the fine morning, (liquid is done rear) can gather in 48 hours after the dispenser;
(3) extract test sample:
Spray continuously three days the first week at unification in the 4th day sample of gathering, randomly draw plant as for the examination material, allow their blade of rear collection be test sample;
(4) carry out the processing of different washing agent and different soak times:
The processing of 4 levels is set, in order to keep the consistance of sample, reduces experimental error, 4 processing are carried out simultaneously; Respectively rape is placed clear water, detersive, salt solution, rice washing water to soak; The time of each horizontal processing is followed successively by 5min, 15min, 30min, 60min, 120min, 6 processing of blank (CK); Wherein, blank (CK) refers to that rape is without immersion treatment.
(5) preparation of reference substance and test solution:
The preparation of reference substance solution: rape leaf shredded be placed in the mortar, after fully grinding, accurately take by weighing the 5.00g stamping in centrifuge tube, make a record, add subsequently the 15mL hexane extract, place in the supersonic wave cleaning machine behind the ultrasonic extraction 15min, in hydro-extractor with 3000rmin
-1The centrifugal 8min of rotating speed;
Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters the 250mL round-bottomed flask, washs the funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the flask; Be concentrated into 2mL with Rotary Evaporators, concentrate is settled to 5mL with normal hexane, namely gets reference substance solution.
The preparation of sample solution: after rape carried out the different time immersion treatment, from soak solution, pull out, place mortar, after fully grinding, accurately take by weighing the 5.00g stamping in centrifuge tube, make a record, add subsequently the 15mL hexane extract, place in the supersonic wave cleaning machine behind the ultrasonic extraction 15min, in hydro-extractor with 3000rmin
-1The centrifugal 8min of rotating speed; Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters the 250mL round-bottomed flask, washs the funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the flask; Be concentrated into 2mL with Rotary Evaporators, concentrate is settled to 5mL with normal hexane, namely gets sample solution.
(6) determination method:
Accurate reference substance solution and the need testing solution inject gas chromatograph drawn measured respectively, calculates the content of test sample Chlorpyrifos Residue by the peak area of calculation sample chromatogram.The detersive that its result processes comparison diagrams, Fig. 2 such as 6 of the clear water immersions of Fig. 1 soaks lower 6 the processing comparison diagrams of saline sook of lower 6 processing comparison diagrams, Fig. 3, the rice washing waters of Fig. 4 soak shown in lower 6 processing comparison diagrams.
Carry out statistical study by the residual content of chlopyrifos farming that clear water, detersive, salt solution, four kinds of cleaning materials of rice washing water were processed after 5 minutes, comparison diagram was respectively processed in the immersion that draws Fig. 5 in 5 minutes.
Carry out statistical study by clear water, detersive, salt solution, four kinds of cleaning materials of rice washing water being carried out processed the residual content of rear chlopyrifos farming in 15 minutes, comparison diagram was respectively processed in the immersion that draws Fig. 6 in 15 minutes.
Contrast by Fig. 1～Fig. 6 can be found out, soaks with detersive, and adhering to of agricultural chemicals is more effective for reducing.It is undesirable to use rice washing water and saline sook to process the residual reduction effect of chlopyrifos farming, and the time should not be longer than 60min.With clear water the rape immersion is washed by rubbing with the hands after 10～60 minutes more a little, just can remove 15%～60% residues of pesticides.
The detection method of the embodiment of the invention can detect which kind of cleaning way of affirmation and can effectively remove chlopyrifos residual in the rape, thereby find a kind of better cleaning rape to remove the method for its chlopyrifos residue.The vapor-phase chromatography that adopts among the present invention, chromatography different from the past, degraded enzyme process, chemiluminescence and biosensor technique have the separation efficiency height, and the characteristics such as highly sensitive, analysis speed is fast, applied range have guaranteed the accurate of testing result.Can clearly draw easily different modes and clean the flat situation about changing of rear rape Chlorpyrifos Residue water gaging, thereby determine which kind of cleaning way more can effectively reduce the residual chlopyrifos in the rape, can be the guidance that people's daily life provides the edible aspect of vegetable safety.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (6)
1. the detection method to the difference of residual chlopyrifos in the rape after the different modes cleaning is characterized in that, comprising:
After will gathering with the rape that chlopyrifos is processed, randomly draw rapeseed plants, get the blade of described rapeseed plants as sample;
Choosing different cleaning ways cleans described sample, after the cleaning described sample is made sample solution, described sample solution is carried out gas chromatographic analysis with reference substance solution by vapor-phase chromatography respectively, draw the difference of chlopyrifos content by calculating the spectrum peak area ratio.
2. method according to claim 1 is characterized in that, described different cleaning way comprises:
Clear water soaking and washing, saline sook cleaning, rice washing water soaking and washing or detersive soaking and washing.
3. method according to claim 2 is characterized in that, the soak time of described each soaking and washing mode is respectively:
5 minutes, 15 minutes, 30 minutes, 60 minutes, 120 minutes.
4. method according to claim 1 is characterized in that, the described sample after will cleaning is in the following manner made sample solution, comprising:
Described sample after cleaning shredded be placed in the mortar, after fully grinding, take by weighing the 5g stamping in centrifuge tube, add the 15mL hexane extract, place in the supersonic wave cleaning machine ultrasonic extraction after 15 minutes, in hydro-extractor with 3000rmin
-1Centrifugal 8 minutes of rotating speed; Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters round-bottomed flask, washs the glass funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the round-bottomed flask; With Rotary Evaporators the solution in the described round-bottomed flask is condensed into the 2mL concentrate, described concentrate is settled to 5mL with normal hexane, namely gets sample solution.
5. method according to claim 1 is characterized in that, described reference substance solution prepares in the following manner, comprising:
Rape leaf shredded be placed in the mortar, after fully grinding, take by weighing the 5g stamping in centrifuge tube, add the 15mL hexane extract, place in the supersonic wave cleaning machine ultrasonic extraction after 15 minutes, in hydro-extractor with 3000rmin
-1Centrifugal 8 minutes of rotating speed;
Through the glass funnel dehydration of anhydrous sodium sulfate is housed, filter enters round-bottomed flask, washs the funnel that anhydrous sodium sulfate is housed with normal hexane with the supernatant after centrifugal, and cleansing solution is also incorporated in the described round-bottomed flask; With Rotary Evaporators the solution in the described round-bottomed flask is condensed into the 2mL concentrate, described concentrate is settled to 5mL with normal hexane, namely gets reference substance solution.
6. method according to claim 1 is characterized in that, the plucking time of the blade of described rapeseed plants as sample is no more than 1 hour.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101116460A (en) * | 2007-08-30 | 2008-02-06 | 宜昌萧氏茶叶集团有限公司 | Method for cleaning fresh tea leaf |
| CN102121930A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Treatment method used before measurement of sample containing abamectin and chlorpyrifos |
| CN102423019A (en) * | 2011-11-17 | 2012-04-25 | 宁波海通食品科技有限公司 | Physical and chemical treatment method for degradation of specific pesticide-containing vegetable raw material before processing, and quality guaranteeing |
-
2012
- 2012-11-29 CN CN2012105009484A patent/CN102967673A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101116460A (en) * | 2007-08-30 | 2008-02-06 | 宜昌萧氏茶叶集团有限公司 | Method for cleaning fresh tea leaf |
| CN102121930A (en) * | 2010-12-20 | 2011-07-13 | 天津市农业科学院中心实验室 | Treatment method used before measurement of sample containing abamectin and chlorpyrifos |
| CN102423019A (en) * | 2011-11-17 | 2012-04-25 | 宁波海通食品科技有限公司 | Physical and chemical treatment method for degradation of specific pesticide-containing vegetable raw material before processing, and quality guaranteeing |
Non-Patent Citations (7)
| Title |
|---|
| 《现代农药》 20020210 汪军 GC-MS定性定量分析出口西兰花样品中毒死蜱的农药残留量 , 第1期 * |
| ZHI-YONG ZHANG ET AL.: "Effects of home preparation on pesticide residues in cabbage", 《FOOD CONTROL》, vol. 18, no. 12, 31 December 2007 (2007-12-31) * |
| 刘振龙 等: "小白菜中毒死蜱残留去除方法的研究", 《农业环境科学学报》, vol. 26, no. 2, 20 March 2007 (2007-03-20) * |
| 张锐 等: "不同洗涤处理对叶菜中农药残留去除效果比较", 《农业科技与装备》, no. 5, 31 May 2010 (2010-05-31) * |
| 林旭 等: "不同清洗方式对香菇中毒死蜱残留去除效果的研究", 《安徽农业大学学报》, vol. 39, no. 1, 26 December 2011 (2011-12-26) * |
| 汪军: "GC—MS定性定量分析出口西兰花样品中毒死蜱的农药残留量", 《现代农药》, no. 1, 10 February 2002 (2002-02-10) * |
| 王向未 等: "不同加工方式对豇豆中毒死蜱残留量的影响", 《食品工业科技》, vol. 33, no. 16, 31 March 2012 (2012-03-31) * |
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