CN101793879A - Method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides - Google Patents

Method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides Download PDF

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Publication number
CN101793879A
CN101793879A CN201010106204A CN201010106204A CN101793879A CN 101793879 A CN101793879 A CN 101793879A CN 201010106204 A CN201010106204 A CN 201010106204A CN 201010106204 A CN201010106204 A CN 201010106204A CN 101793879 A CN101793879 A CN 101793879A
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Prior art keywords
residues
sample
measuring
mixed liquor
extract
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CN201010106204A
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Chinese (zh)
Inventor
宋春满
方敦煌
丁元明
旦有明
师君丽
唐旭兵
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Yunnan Academy of Tobacco Agricultural Sciences
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Yunnan Academy of Tobacco Agricultural Sciences
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Priority to CN201010106204A priority Critical patent/CN101793879A/en
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Abstract

The invention discloses a method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides. The method comprises the following working procedures: crushing a tobacco sample until grain diameters are less than 450 mu m; adding 10 to 20ml of extracting solution and internal standard solution into every program of tobacco sample; extracting the mixed solution by using ultrasonic wave; filtering the mixed solution by using a funnel filled with anhydrous sodium sulfate to obtain the extracting solution; adding the extracting solution into a Florisil solid extraction column for extracting and eluting; collecting an eluent; analyzing the eluent by using a gas chromatograph, wherein the analysis comprises the following conditions: adopting an Elite 5MS capillary column, high-purity N2 as a carrier gas, a constant flow mode in which the flow rate is 0.5 to 1.5 ml/min, a sample inlet temperature of between 280 and 320 DEG C, a detector temperature of between 330 and 370 DEG C, splitless sampling in which the sampling volume is between 1 and 2 mu L, and an initial temperature of 100 DEG C which rises from 100 to 180 DEG C at a speed of 8 DEG C/min, is kept for 4 minutes, rises from 180 to 270 DEG C at the speed of 5 DEG C/min and is kept for 15 minutes until all sample flows out completely; and determining the nature of the sample by using the retaining time of a standard sample and quantifying by using an internal standard method. In the method, ultrasonic wave is adopted for extracting and a solid extraction column is adopted for purifying, so that the method has the advantages of operating step simplification, high work efficiency, good purification effect, capability of simultaneously measuring multiple residues of 25 kinds of pesticides including 17 organic chloride pesticides of hexachlorocyclohexane, DDT and the like, seven pyrethroid pesticides such as fenpropathrin and the like, and one plant growth regulator.

Description

Measure the method for organochlorine class and pyrethroid pesticide multiple residues simultaneously
Technical field
The invention belongs to the Analytical Techniques of Pesticide Residues field, be specifically related to a kind of method of measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously.
Background technology
Although organochlorine insecticides is not recommended or is forbidden using on tobacco, pyrethroid insecticides is to recommend to use a bit, but the residual tobacco residues of pesticides of relatively paying close attention in domestic and international tobacco and the tobacco product that remain of organochlorine class and pyrethroid insecticides.Therefore, this two pesticide residue is all set up the method for standard both at home and abroad, method as organochlorine insecticide retention analysis in tobacco and the tobacco product has " the mensuration vapor-phase chromatography of GB/T13596-2004 tobacco and tobacco product Residual Levels of Organochlorine Pesticides ", and the method for pyrethroid insecticides retention analysis has " mensuration of GB/T 13595-2004 tobacco and tobacco product pyrethroid insectide, organophosphorus insecticide, nitrogenous persticide residue " etc.These two standards can only be to organochlorine class in tobacco and the tobacco product, pyrethroid insecticides is residual measures respectively, and can not measure simultaneously.Up to the present, yet there are no the method for measuring organochlorine class and pyrethroid insecticides multiple residues simultaneously.Therefore the efficient of prior art mensuration organochlorine and pyrethroid insecticides multiple residues is low, the time is long, cost is high.
Summary of the invention
The objective of the invention is to overcome the deficiency that prior art can not be measured organochlorine class and pyrethroid pesticide multiple residues simultaneously, measure the method for organochlorine class and pyrethroid pesticide multiple residues when a kind of easy, quick, highly sensitive, instrument highly versatile is provided.
Purpose of the present invention realizes that like this technical scheme comprises following operation:
A, cigarette sample make particle diameter less than 450 μ m through pulverizing, by amount adding extract and the interior mark liquid of every gram cigarette sample 10~20ml, and Extraction by Ultrasound, the funnel through anhydrous sodium sulfate is housed filters, the acquisition extract;
B, extract add to the Florisil column solid phase extraction, and wash-out is collected eluent;
Elite 5MS capillary column is adopted in the gas chromatograph analysis of C, eluent; Carrier gas is a high-purity N 2Current constant mode, flow velocity 0.5~1.5ml/min; 280~320 ℃ of injector temperatures, 330~370 ℃ of detector temperatures; Split sampling not, sample size 1~2 μ L; 100 ℃ of initial temperature rise to 180 ℃ with 8 ℃/min by 100 ℃, keep 4min, rise to 270 ℃ with 5 ℃/min by 180 ℃ again, keep 15min all to flow out to sample;
The retention time of D, employing standard items is carried out qualitative, inner mark method ration.
The present invention adopts Extraction by Ultrasound, solid-phase extraction column to purify, simplified operation steps, high efficiency, good purification can be measured 7 kinds of pyrethroid insecticideses such as 17 kinds of organochlorine classes such as benzene hexachloride, DDT and Fenpropathrin and the flumetralim 1 plant growth regulators multiple residues of totally 25 kinds of agricultural chemicals simultaneously.Recovery height of the present invention, good reproducibility can satisfy multiple residues and analyze requirement.
Description of drawings
Fig. 1 adds the tobacco sample chromatogram of organochlorine and pyrethroid pesticide standard items for inventive method;
Fig. 2 is blank tobacco sample chromatogram.
Among the figure: 1, α-BHC, 2, hexachloro-benzene, 3, β-BHC, 4, γ-BHC, 5, δ-BHC, 6, heptachlor, 7, drinox, 8, Heptachlor epoxide A, 9, Heptachlor epoxide B, 10, Niran, 11, o, p '-DDE, 12, flumetralim, 13, α-5a,6,9,9a-hexahydro-6,9-methano-2,4,14, dieldrite, 15, p, p '-DDE, 16, o, p '-DDD, 17, p, p '-DDD, 18, o, p '-DDT, 19, p, p '-DDT, 20, Fenpropathrin, 21, interior mark, 22, betacyfluthrin, 23, Permethrin A, 24, Permethrin B, 25, cyfloxylate A, 26, cyfloxylate B, 27, cyfloxylate C, 28, cyfloxylate D, 29, cypermethrin A, 30, cypermethrin B, 31, cypermethrin C, 32, cypermethrin D, 33, fenvalerate, 34, cis fenvalerate, 35, decis.
Embodiment
The invention will be further described below in conjunction with accompanying drawing and embodiment, but never in any form the present invention is limited, and anyly all belongs to protection scope of the present invention based on the conversion that the present invention did.
Technical solution of the present invention comprises following operation:
A, cigarette sample make particle diameter less than 450 μ m through pulverizing, by amount adding extract and the interior mark liquid of every gram cigarette sample 10~20ml, and Extraction by Ultrasound, the funnel through anhydrous sodium sulfate is housed filters, the acquisition extract;
B, extract add to the Florisil column solid phase extraction, and wash-out is collected eluent;
Elite 5MS capillary column is adopted in the gas chromatograph analysis of C, eluent; Carrier gas is a high-purity N 2Current constant mode, flow velocity 0.5~1.5ml/min; 280~320 ℃ of injector temperatures, 330~370 ℃ of detector temperatures; Split sampling not, sample size 1~2 μ L; 100 ℃ of initial temperature rise to 180 ℃ with 8 ℃/min by 100 ℃, keep 4min, rise to 270 ℃ with 5 ℃/min by 180 ℃ again, keep 15min all to flow out to sample;
The retention time of D, employing standard items is carried out qualitative, inner mark method ration.
Described extract is a normal hexane: acetonitrile mixed liquor (V: V=1: 1), or normal hexane: ethyl acetate mixed liquor (V: V=1: 1), or normal hexane: acetone mixed liquor (V: V=1: 1), or normal hexane: methylene chloride mixed liquor (V: V=1: 1), or normal hexane: methyl alcohol mixed liquor (V: V=1: 1), or acetonitrile: methylene chloride mixed liquor (V: V=1: 1).
Be designated as ten dichloro-octahydros-1,3 in described, 4-methine-1H-ring fourth is (c, d) dicyclopentadiene (mirex), or 2,4,5,6-tetrachloro m-xylene, or ten chlordiphenyls also.
Described ultrasonic Extraction adopts extract to soak 1h, ultrasonic Extraction 10~15min; Or ultrasonic Extraction 30~45min.
The eluent of described C operation under same chromatographic condition, with same ECD detecting device, is measured 25 kinds of pesticide residues with the gas chromatograph analysis simultaneously.
Be illustrated below by experimental data.
Take by weighing 2.0g be crushed to particle diameter less than the cigarette sample of 450 μ m in 50ml scale test tube, add organochlorine class and pyrethroid insecticides standard specimen, make 17 kinds of organochlorine insecticides content in the tobacco leaf reach 0.05 μ g/g, 7 kinds of pyrethroid insecticideses and 1 plant growth regulators content and reach 0.5 μ g/g, add 20ml normal hexane-acetonitrile mixed liquor (V: V=1: 1) reach interior mark liquid ultrasonic Extraction 30min again, leave standstill, filter to flask through the funnel that anhydrous sodium sulfate is housed and purify.Extract adds to Florisil column solid phase extraction post (500mg/6ml, the Agilent product), uses 3ml normal hexane, 3ml acetonitrile pre-leaching Florisil solid-phase extraction column respectively, add extract, with 1: 1 normal hexane-acetonitrile mixed liquor 5ml wash-out, eluent is analyzed with gas chromatograph.Analysis condition: adopt PerkinElmer Clarus 500GC (joining ECD) gas chromatograph, chromatographic column: Elite 5MS (30m * 0.25mm * 0.25 μ m, PE company product) capillary column; Carrier gas: high-purity N 2, current constant mode, flow velocity: 1ml/min; 300 ℃ of injector temperatures, 350 ℃ of detector temperatures; Split sampling not, sample size 2 μ L.The column temperature program: 100 ℃ of initial temperature, rise to 180 ℃ with 8 ℃/min by 100 ℃, keep 4min, rise to 270 ℃ with 5 ℃/min by 180 ℃ again, keep 15min all to flow out to sample.
The retention time of employing standard items is carried out qualitative, and with ten dichloro-octahydros-1,3, also (c, mark carried out quantitative test to 4-methine-1H-ring fourth in d) dicyclopentadiene (mirex) was done.
Under above-mentioned experiment condition, interior mark and each component compound separation be (seeing accompanying drawing 1) fully, can carry out qualitative, quantitative test to these components.By chromatogram (seeing accompanying drawing 1,2) as can be known, noiseless peak, the peak shape symmetry is sharp-pointed, signal is strong, signal to noise ratio (S/N ratio) is high.
With the normal hexane is solvent, prepare serial mixed standard solution respectively, wherein organochlorine concentration is 0.01,0.02,0.03,0.04,0.05,0.06,0.07,0.08,0.09,0.10 μ g/mL, corresponding pyrethroid pesticide and plant growth regulator concentration are 0.10,0.20,0.30,0.40,0.50,0.60,0.70,0.80,0.90,1.00 μ g/mL, totally 10 mixed standard solutions, under above-mentioned chromatographic condition, carry out stratographic analysis, adopt the retention time of standard items qualitative, ten dichloro-octahydros-1,3,4-methine-1H-ring fourth is (c also, d) scalar quantity in dicyclopentadiene (mirex) is done, the linear relationship of each component, related coefficient, detection limit sees Table 1, shows the detection method sensitivity.
Table 1 each component linear relationship and detection limit
Select tobacco sample for use, add the organochlorine class respectively and the cinerins agricultural chemicals carries out recovery test, repeat 6 parallel laboratory tests, the results are shown in Table 2, the each component recovery 83.28%~102.33%, relative standard deviation 2.85%~5.44% illustrates that this method has the recovery and precision preferably to 17 kinds of organochlorine insecticideses, 7 kinds of pyrethroid insecticideses and 1 plant growth regulators are residual, can satisfy multiple residues and analyze requirement.
The recovery of table 2 method and precision
The present invention has following characteristics:
1, the employing ultrasonic wave extracts, the commercialization solid-phase extraction column purifies, qualitative, the inner mark method ration of retention time of standard sample of pesticide, only being equipped with general ECD detector with gas chromatograph just can directly detect, relative GC-MS, instrument operating cost is lower, instrumentation is easier, and versatility is stronger.
2, simplified operating procedure, efficient height, good purification, can measure simultaneously 7 kinds of pyrethroid insecticideses such as 17 kinds of organochlorine classes such as BHC, DDT and Fenpropathrin and the flumetralim 1 Plants growth regulator multiple residues of totally 25 kinds of agricultural chemicals, the rate of recovery 83.28%~102.33%, relative standard deviation 2.85%~5.44% can satisfy multiple residues and analyze requirement.

Claims (5)

1. method of measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously is characterized in that comprising following operation:
A, cigarette sample make particle diameter less than 450 μ m through pulverizing, by amount adding extract and the interior mark liquid of every gram cigarette sample 10~20ml, and Extraction by Ultrasound, the funnel through anhydrous sodium sulfate is housed filters, the acquisition extract;
B, extract add to the Florisil column solid phase extraction, and wash-out is collected eluent;
Elite 5MS capillary column is adopted in the gas chromatograph analysis of C, eluent; Carrier gas is a high-purity N 2Current constant mode, flow velocity 0.5~1.5ml/min; 280~320 ℃ of injector temperatures, 330~370 ℃ of detector temperatures; Split sampling not, sample size 1~2 μ L; 100 ℃ of initial temperature rise to 180 ℃ with 8 ℃/min by 100 ℃, keep 4min, rise to 270 ℃ with 5 ℃/min by 180 ℃ again, keep 15min all to flow out to sample;
The retention time of D, employing standard items is carried out qualitative, inner mark method ration.
2. the method for measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously as claimed in claim 1, it is characterized in that: described extract is a normal hexane: acetonitrile mixed liquor (V: V=1: 1), or normal hexane: ethyl acetate mixed liquor (V: V=1: 1), or normal hexane: acetone mixed liquor (V: V=1: 1), or normal hexane: methylene chloride mixed liquor (V: V=1: 1), or normal hexane: methyl alcohol mixed liquor (V: V=1: 1), or acetonitrile: methylene chloride mixed liquor (V: V=1: 1).
3. the method for measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously as claimed in claim 1, it is characterized in that: be designated as ten dichloro-octahydros-1 in described, 3,4-methine-1H-ring fourth is (c, d) dicyclopentadiene (mirex), or 2 also, 4,5,6-tetrachloro m-xylene, or ten chlordiphenyls.
4. the method for measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously as claimed in claim 1 is characterized in that: described ultrasonic Extraction adopts extract to soak 1h, ultrasonic Extraction 10~15min; Or ultrasonic Extraction 30~45min.
5. the method for measuring organochlorine class and pyrethroid pesticide multiple residues simultaneously as claimed in claim 1, it is characterized in that: the eluent of described C operation with the gas chromatograph analysis under same chromatographic condition, with same ECD detecting device, measure 25 kinds of pesticide residues simultaneously.
CN201010106204A 2010-02-05 2010-02-05 Method for simultaneously measuring multiple residues of organic chloride and pyrethroid pesticides Pending CN101793879A (en)

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Cited By (17)

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Publication number Priority date Publication date Assignee Title
CN102002367A (en) * 2010-11-17 2011-04-06 中国科学院南京土壤研究所 Eluent for soil polluted by organochlorine pesticides and repair method by using same
CN102288715A (en) * 2011-07-21 2011-12-21 广东出入境检验检疫局检验检疫技术中心 Method for detecting mirex content of rubber part of electronic/electric product
CN102998407A (en) * 2012-12-04 2013-03-27 漳州片仔癀药业股份有限公司 Method for detecting pesticide residues in anti-inflammatory and analgesic bolus
CN103175918A (en) * 2013-02-26 2013-06-26 福建中烟工业有限责任公司 Method for extracting and detecting organic chloride pesticide residues in tobaccos and tobacco products by using ultrasonic solvent
CN103257198A (en) * 2013-06-08 2013-08-21 国家烟草质量监督检验中心 GC-MS/MS (Gas Chromatography-Mass Spectrometer) method for analyzing organo-chlorine pesticide residues in tobacco and tobacco products
CN103293267A (en) * 2013-06-08 2013-09-11 国家烟草质量监督检验中心 GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product
CN103913528A (en) * 2014-04-24 2014-07-09 江苏太湖地区农业科学研究所 Quantitative detection method for pyrethriods pesticides in fresh tea
CN103926362A (en) * 2014-04-24 2014-07-16 江苏太湖地区农业科学研究所 Quantitative detection method for pyrethriods pesticide in soil
CN103995074A (en) * 2014-04-18 2014-08-20 北京三元食品股份有限公司 Method for detecting residual quantity of organochlorine pesticides in raw milk
CN106546584A (en) * 2016-11-09 2017-03-29 百奥森(江苏)食品安全科技有限公司 The quick detection kit and using method of organochlorine residue in a kind of agricultural product
CN106645465A (en) * 2016-11-29 2017-05-10 保山市质量技术监督综合检测中心 Method for determining organochlorine and pyrethroid pesticide residues in fresh Dendrobium strips
CN108037218A (en) * 2018-01-22 2018-05-15 淮安出入境检验检疫局综合技术服务中心 The method of 5a,6,9,9a-hexahydro-6,9-methano-2,4 in gas chromatography tandem mass spectrometry method measure feed
CN108459112A (en) * 2018-05-18 2018-08-28 中国水产科学研究院淡水渔业研究中心 The detection method of Organochlorine Pesticides in Eriocheir sinensis crab cream
CN108802228A (en) * 2018-06-20 2018-11-13 苏州出入境检验检疫局检验检疫综合技术中心 The remaining screening of pesticide and quantitative approach in a kind of cosmetics and its raw material
CN109142550A (en) * 2017-06-15 2019-01-04 中国科学院大连化学物理研究所 A kind of research method of plant instruction soil persistance organic chloride pollution
CN109655538A (en) * 2018-12-12 2019-04-19 浙江方圆检测集团股份有限公司 Method that is a kind of while detecting Polychlorinated biphenyls and phthalic acid ester in milk powder
CN109975458A (en) * 2019-04-22 2019-07-05 河南中测技术检测服务有限公司 Method that is a kind of while detecting sitotoxismus dead tick and procymidone

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Cited By (24)

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Publication number Priority date Publication date Assignee Title
CN102002367A (en) * 2010-11-17 2011-04-06 中国科学院南京土壤研究所 Eluent for soil polluted by organochlorine pesticides and repair method by using same
CN102288715A (en) * 2011-07-21 2011-12-21 广东出入境检验检疫局检验检疫技术中心 Method for detecting mirex content of rubber part of electronic/electric product
CN102288715B (en) * 2011-07-21 2014-03-12 广东出入境检验检疫局检验检疫技术中心 Method for detecting mirex content of rubber part of electronic/electric product
CN102998407B (en) * 2012-12-04 2015-03-18 漳州片仔癀药业股份有限公司 Method for detecting pesticide residues in anti-inflammatory and analgesic bolus
CN102998407A (en) * 2012-12-04 2013-03-27 漳州片仔癀药业股份有限公司 Method for detecting pesticide residues in anti-inflammatory and analgesic bolus
CN103175918A (en) * 2013-02-26 2013-06-26 福建中烟工业有限责任公司 Method for extracting and detecting organic chloride pesticide residues in tobaccos and tobacco products by using ultrasonic solvent
CN103257198A (en) * 2013-06-08 2013-08-21 国家烟草质量监督检验中心 GC-MS/MS (Gas Chromatography-Mass Spectrometer) method for analyzing organo-chlorine pesticide residues in tobacco and tobacco products
CN103257198B (en) * 2013-06-08 2014-09-10 国家烟草质量监督检验中心 GC-MS/MS (Gas Chromatography-Mass Spectrometer) method for analyzing organo-chlorine pesticide residues in tobacco and tobacco products
CN103293267A (en) * 2013-06-08 2013-09-11 国家烟草质量监督检验中心 GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product
CN103995074A (en) * 2014-04-18 2014-08-20 北京三元食品股份有限公司 Method for detecting residual quantity of organochlorine pesticides in raw milk
CN103913528A (en) * 2014-04-24 2014-07-09 江苏太湖地区农业科学研究所 Quantitative detection method for pyrethriods pesticides in fresh tea
CN103926362A (en) * 2014-04-24 2014-07-16 江苏太湖地区农业科学研究所 Quantitative detection method for pyrethriods pesticide in soil
CN103926362B (en) * 2014-04-24 2015-11-25 江苏太湖地区农业科学研究所 The quantitative detecting method of pyrethroid pesticide in a kind of soil
CN103913528B (en) * 2014-04-24 2015-04-29 江苏太湖地区农业科学研究所 Quantitative detection method for pyrethriods pesticides in fresh tea
CN106546584A (en) * 2016-11-09 2017-03-29 百奥森(江苏)食品安全科技有限公司 The quick detection kit and using method of organochlorine residue in a kind of agricultural product
CN106645465A (en) * 2016-11-29 2017-05-10 保山市质量技术监督综合检测中心 Method for determining organochlorine and pyrethroid pesticide residues in fresh Dendrobium strips
CN109142550A (en) * 2017-06-15 2019-01-04 中国科学院大连化学物理研究所 A kind of research method of plant instruction soil persistance organic chloride pollution
CN108037218A (en) * 2018-01-22 2018-05-15 淮安出入境检验检疫局综合技术服务中心 The method of 5a,6,9,9a-hexahydro-6,9-methano-2,4 in gas chromatography tandem mass spectrometry method measure feed
CN108459112A (en) * 2018-05-18 2018-08-28 中国水产科学研究院淡水渔业研究中心 The detection method of Organochlorine Pesticides in Eriocheir sinensis crab cream
CN108459112B (en) * 2018-05-18 2020-12-29 中国水产科学研究院淡水渔业研究中心 Method for detecting content of organochlorine pesticide in crab cream of Eriocheir sinensis
CN108802228A (en) * 2018-06-20 2018-11-13 苏州出入境检验检疫局检验检疫综合技术中心 The remaining screening of pesticide and quantitative approach in a kind of cosmetics and its raw material
CN109655538A (en) * 2018-12-12 2019-04-19 浙江方圆检测集团股份有限公司 Method that is a kind of while detecting Polychlorinated biphenyls and phthalic acid ester in milk powder
CN109655538B (en) * 2018-12-12 2021-09-21 浙江方圆检测集团股份有限公司 Method for simultaneously detecting polychlorinated biphenyl and phthalic acid ester in milk powder
CN109975458A (en) * 2019-04-22 2019-07-05 河南中测技术检测服务有限公司 Method that is a kind of while detecting sitotoxismus dead tick and procymidone

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Application publication date: 20100804