Determination of 14 Organophosphorus Pesticide Residues in Mutton by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry(GPC-GC-MS)

[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.

Determination of Eight Organophosphorus Pesticide Residues in Pepper by QuEChERS-Gas Chromatography

[ Objectives] This study was conducted to establish a QuEChERS-gas chromatography method for determination of eight kinds of organophosphorus pesticide residues in pepper. [Methods] The samples were extracted by acetonitrile, and anhydrous magnesium sulfate was used for salting out. The extracts were then purified by dispersive solid phase extraction combining with GCB, C18 and PSA. Samples were analyzed by FPD detector. External standard was used as quantitive method. [ Results] The detection limits were in the range of 0. 001 -0. 008 mg/kg, the average recoveries ranged from 83.5% to 101.2% , and the relative standard deviation （RSD） of the eight organophosphorus pesticide residues were below 5%. [ Conclusions] The method is simple, quick, easy and effective for the determination of pepper.

Research on Comparison of Gas Chromatography and Liquid Chromatogram Detecting Pesticide Residue

The existing methods of detecting pesticide residue include gas chromatography, high performance liquid chromatography, gas chromatograph-mass, liquid chromatograph-mass, capillary electrophoresis, radioimmunoassay, biosensor and rapid detection on the spot. The paper analyzes the comparison of gas chromatography and liquid chromatogram detecting pesticide residue, for achieving the development tendency and the future goal of analyzing pesticide residue.

Study on Detection of Organochlorine Pesticide Residue in Ginseng

To investigate the residue situation of pesticides in ginseng, total 17 samples of ginseng-growing soil, ginseng roots and ginseng seeds were collected from 5 regions of Fusong County, and the contents of organochlorine pesticide residues in the samples were detected by using ultrasonic-assisted extraction and gas chromatography with acetone-ligroin as the solvent, thereby providing suitable recommendations and scientific basis for the selection of ginseng-growing soil.

Rapid Determination of Pesticide Residues in Fresh Sweet Corn

Objective] This study aimed to detect al organophosphate, organochlorine and pyrethroid pesticide residues in fresh sweet corn in one determination using a gas chromatograph. [Method] The pesticide residues in fresh sweet corn were ex-tracted and loaded to simultaneously the gas chromatograph Agilent 6890N which was equipped with two autosamplers, two columns and two detectors. [Result] Al the 26 pesticides were completely separated and eluted out within 25 min. The re-coveries of standard addition of the 26 pesticides ranged from 76% to 106%, with relative standard deviations （RSD） ranging from 0.5% to 8.9%. The linear regression equation fit wel from 0.050 to 1.500 mg/L corn extract （r2＆gt;0.996）. [Conclusion] The method is accuracy, which meets the requirements of pesticide residue analysis and can be used for the rapid detection, qualitative and quantitative analysis of pesticide residues in fresh sweet corn.

Determination of Organochlorine and Synthetic Pyrethroid Pesticide Residues in Water Samples Collected from Different Locations of Bangladesh

The present study was aimed to validate an analytical method for the quantification of 19 organochlorine and 2 synthetic pyrethroid pesticide residues in water samples using modified quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and Gas Chromatography coupled with Electron Capture Detector (ECD). The selected pesticide residues were determined by in-house validated method. The analytical method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 78% to 117% with RSDr ≤ 12% in two fortification levels of 0.02 and 0.1 mg/L. The linearity was ≥0.995 for all of the selected pesticides. The LOD ranged from 0.003 to 0.006 mg/L and the LOQ was 0.02 mg/L for all the selected analytes. This method was applied satisfactorily for the residue analysis of 108 water samples collected from nine districts of Bangladesh. Among the analyzed samples, only 4 had cypermethrin residues (0.026 mg/L, 0.034 mg/L, 0.045 mg/L and 0.05 mg/L). The level of detected cypermethrin residues were above the WHO recommended guide line values of water quality.

Matrix Effects of Fourteen Organophosphorus Pesticides Residues in Nine Kinds of Vegetable Matrices

The matrix effects of 14 organophosphorus pesticides in 9 kinds of vegetables matrices were preliminarily studied by gas chromatography/flame photomet- ric detection（FPD） in the paper. The matrix effects of 14 organophosphoms pesticides in 9 kinds of vegetable matrices at 0.05, 0.1 and 0.2 mg/L were compared, respectively. The results showed that matrix enhancement effect and matrix attenuation effect existed in all cases, while matrix effects did not have strong correlation with concentrations of pesticides, but were related to species of vegetables and structure and polarity of pesticides.

Multi-Residue Levels of Persistent Organochlorine Pesticides in Edible Vegetables: A Human Health Risk Assessment

Background: This study evaluates the quantitative assessment of persistent organochorine pesticide (OCPs) residues in vegetables (Senecio biafrae) from four selected cocoa plantations in Ekiti State, Nigeria. Methods: The pesticides were extracted from the vegetable samples by using USEPA 3500C method and later clean-up on activated silica gel. The pesticides residues in the samples were determined using Gas Chromatography coupled with Electron Capture Detector (GC-ECD). Results: The results showed that the analyzed samples were contaminated with ten OCPs. The mean OCPs concentration ranged from ND—0.399 mg/kg to ND—0.379 mg/kg during the wet and dry seasons respectively. α-BHC, β-BHC, p, p’-DDE, dieldrin, endrin, endosulfan sulphate and methoxychlor were not detected in the samples. Pesticides such as aldrin, endosulfan II, endrin aldehyde and heptachlor slightly exceeded their maximum residue limit. Conclusion: The hazard indices (HI) of heptachlor, endosulfan I, endosulfan II, aldrin, heptachlor-epoxide and p, p’-DDT exceeded 1 and thus pose likely potential non-carcinogenic health risk.

毛细管气相色谱法测定5种中草药中有机氯农药的残留量

建立了怀牛夕等 5种中草药中六六六及滴滴涕异构体含量的气相色谱分析方法。样品以石油醚 +丙酮在索氏提取器中提取 ,提取液以浓硫酸净化。采用SE 30弹性石英毛细管柱分离样品 ,GC ECD检测六六六、滴滴涕农药的残留量。方法的线性范围为 5 .7× 10 - 7～ 2 .8× 10 - 4μg ;最小检测量为 1.3× 10 - 1 4～ 2 .5×10 - 1 2 g ;加样平均回收率为 88.8%～ 99.1% ;RSD为 0 .9%～ 5 .3%。

毛细管气相色谱法测定韭菜中13种有机磷农药残留的研究

建立了毛细管气相色谱法测定韭菜中敌敌畏、甲胺磷、乙酰甲胺磷、甲拌磷、氧化乐果、久效磷、乐果、毒死蜱、甲基对硫磷、马拉硫磷、杀螟硫磷、对硫磷和喹硫磷等13种有机磷农药残留的新方法。考察了进样口压力和程序升温速率对色谱分离的影响。试样用乙腈提取,经毛细管气相色谱柱DB-1701（30 m×0.32 mm×0.25μm）分离,FPD检测器测定。当进样口压力为68.9 kPa,程序升温速率为5℃/min时,13种有机磷农药与韭菜基质在30 min内获得有效分离。添标水平为0.05、0.2 mg/kg时的平均回收率为78%-115%,相对标准偏差为2.6%-10.7%,方法检出限（S/N=3）为0.01-0.03 mg/kg,符合农药多残留定性、定量分析技术的要求。

气相色谱法测定茶叶中有机氯类农药残留量

目的:建立毛细管气相色谱法测定茶叶中12种有机氯农药残留量。方法:采用FDA方法提取、硫酸磺化后,以不分流进样方式用DB-1弹性石英毛细管柱经柱程序升温技术分离,并用电子捕获检测器检测,外标法计算含量。结果:三水平的平均回收率为80.1%～103.8%,RSD为0.52%～6.21%;被测样品中均含有不同程度的农药残留。结论:本方法快速、简便、准确、具有良好的通用性,可用于茶叶中12种有机氯农药残留量的测定。

气相色谱氮磷检测器法用于大米和面粉中22种有机磷和有机氮农药多残留检测

选择气相色谱氮磷检测器法检测大米、面粉中22种有机磷和有机氮农药多残留。大米、面粉样品用丙酮/二氯甲烷(1∶1,V/V)提取,二氯甲烷萃取,丙酮定容,GC-NPD检测。结果表明,该方法分离度较好,灵敏度高,方法的最小检出量在5.180×10-12～8.541×10-11g之间。当添加浓度在0.02～2.00mg·kg-1范围时,大米平均添加回收率为71.71%～109.16%,变异系数为1.16%～12.89%;面粉平均添加回收率为73.87%～113.48%,变异系数为1.75%～15.17%。该方法完全符合农药残留量检测的技术要求,是一种快速有效的分析检测方法,适合在实践中推广使用。

黄芪、三七和西洋参中多种有机氯农药残留量分析

目的 :测定黄芪、三七和西洋参中 15种有机氯农药残留量。方法 :样品经混合溶剂超声提取、Florisil硅土柱层析净化后 ,采用毛细管气相色谱 电子捕获检测器分析被测农药。结果和结论 :2水平的平均加标回收率在 77.30 %～ 130 .1% ,RSD为 0 .75 %～ 31.9%。各被测样品中均含有机氯农药残存。

毛细管气相色谱法分析枸杞子及其制剂中有机氯农药残留

目的建立毛细管气相色谱法同时测定枸杞子及其制剂中有机氯农药六六六、滴滴涕、五氯硝基苯等9个组分残留。方法采用SE-54弹性石英毛细管(0.32 mm×30 m,25μm)色谱柱,进样口温度为230℃；检测器温度300℃。不分流进样,程序升温,电子捕获检测器,高纯度氮气为载气,外标法定量。结果9种有机氯农药在1～100μg·L^(-1)内线性关系良好。枸杞子及其制剂中9种有机氯农药的加样回收率为86.8%～108.8%,相对标准偏差为2.24%～7.02%。各种农药的最低检出限范围为0.02～0.15μg·L^(-1)。结论该方法操作简便、快速、灵敏、准确,适于批量样品的测定。

中药中有机磷农药残留量的毛细管气相色谱测定方法

建立了同时测定中药中8种有机磷农药残留量的前处理及其毛细管气相色谱测定法 ,选用氮磷检测器和SPB -1701毛细管柱,以丙酮 -石油醚混合溶剂提取残留农药。结果表明 :敌百虫、敌敌畏、甲胺磷、二嗪农、乐果、马拉硫磷、甲基对硫磷和对硫磷8种农药在25min内有良好的分离 ;3个不同浓度的标准添加 ,其回收率范围为74.96 %～116.8 % ,相对标准偏差范围为0.71 %～16.91 % ;检出限范围为1.1×10-2～3.36×10-1 pg。该法具有灵敏度高、选择性强、操作简便、重现性好、适用性广等特点 ,有着良好的应用前景。

水果蔬菜中有机磷农药残留量的气相色谱测定方法研究

建立了水果、蔬菜食品中有机磷农药的提取、净化及其毛细管柱气相色谱测定法。用水和丙酮溶剂提取 ,填有无水 Na2 SO4 和Al2 O3的层析柱净化 ,浓缩后采用火焰离子化检测器 (FID)检测到样品中甲胺磷、对硫磷、马拉硫磷、甲基对硫磷的添加回收率分别为81%～ 90 % ,82 %～ 90 % ,84%～ 10 2 % ,80 %～ 90 % ,变异系数均小于8.0 %。实验表明 ,该方法在一定条件下具有灵敏度高 ,净化效果好 ,适用性广等特点 ,可以作为一种常规测定方法。

毛细管气相色谱法分析中药半夏中有机氯农药的残留

采用毛细管气相色谱法测定半夏中8种有机氯农药的残留量。经HP-5石英柱程序升温技术分离,电子捕获检测器检测,外标法计算含量。该方法对8种有机氯农药的平均回收率为85.5%～97.3%;RSD为3.38%～4.56%;本方法快速、简便、准确,具有良好的通用性,可用于半夏中8种有机氯农药残留量的测定。

气相色谱法检测9种药材中有机氯农药的残留量

目的测定9种药材中有机氯农药的残留量。方法以正已烷／丙酮(8／2)混合溶剂,在Florisil固相萃取柱上净化提取,采用毛细管气相色谱柱分离样品和电子捕获检测器进行检测。结果 11种农药能较好地分离,峰面积与其浓度均具有良好线性,两个水平的加样回收率分别为79．9％-89．0％和86．3％-104．8％,相对标准偏差为1．8％-7．1％,检测限为2 g／kg;广藿香和三七中有机氯农药残留超过国家标准。结论所建GC-ECD法能满足药材中有机氯农药残留量的检测, 药典应制订药材中农药残留量的标准。

茶叶中啶虫脒残留量检测方法的研究

建立了啶虫脒在茶叶中残留量的气相色谱检测方法。样品采用丙酮/正已烷(1/2,v/v)混合溶剂提取,经LC-18SPE小柱净化,气相色谱(配ECD)检测,以保留时间和外标法定性、定量。结果表明,该方法的最低检出限为0.004mg/kg,不同水平的加标回收率范围为73.8%～108.7%,RSD(n=6)为8.51%～10.1%。方法操作简便,净化效果理想,能满足残留分析的要求,可用于茶叶啶虫脒残留量的测定。该方法也可为其他产品中啶虫脒残留量的测定提供参考。

凝胶渗透色谱净化-气相色谱测定中成药中有机氯农药的残留量

目的建立凝胶渗透色谱（GPC）净化-毛细管气相色谱测定中成药中有机氯农药残留量的方法。方法凝胶渗透色谱采用的流动相为丙酮-环己烷（1：4），最佳流速是5ml／min，最佳馏分收集时间是15-26min。结果低、中、高3个添加水平的回收率分别为85．5％～115．0％，84．3％～123．4％，86．7％-114．0％，相对标准偏差（RSD）为0．1％．9．3％，检出限0．008—0．05μg／kg。结论该方法简便，分离效果好，灵敏度高，重现性好。