液相色谱—电喷雾串联质谱法测定生姜中215种农药残留
|
摘要
农药是农业生产用于防治病、虫、杂草对农作物危害不可缺少的物质,对促进农业增产有极重要的作用。然而,随着科学技术的发展,化学农药的品种和数量不断增加,因农药的长期大量使用与滥用,农药污染问题经常发生,农药残留对人类健康和环境造成的毒害越来越为人们所关注。生姜不仅是我国人民日常饮食中离不开的调味品和食品,而且也是我国重要的出口创汇蔬菜品种之一。生姜在种植过程中也会发生各种病虫害,为了不影响产量,姜农会对生姜施与各种农药,加上土壤中其它的各类农药,生姜也会遭遇多种农药残留。世界各国对进出口生姜中农药残留的检测项目不断增加,限量标准日趋严格,最大残留限量也大幅度降低,我国出口产品被进口国退回事件时有发生。本文对生姜中农药多残留的提取、净化技术和液相色谱-串联质谱检测条件进行了研究,建立了固相萃取净化、液相色谱-电喷雾串联质谱测定生姜中215种农药多残留的方法。
主要研究结果如下:
1.对实验的提取溶剂、提取方法、净化方式进行了研究,建立了采用1%的醋酸乙腈均质提取、Waters Sep-Pak Vac固相萃取柱净化的方法从生姜中提取净化多种农药残留。
2.液相色谱-串联质谱检测方面,建立了215种农药残留液相色谱-串联质谱检测方法。结果表明,215种农药在相应的质量浓度范围内,各农药的响应值与其质量浓度均成良好的线性范围,215种农药线性相关系数大于0.99的有203个,占总数的94 %。215种农药的最小检出限为0.01~70.45μg/L;最低定量限范围为0.04~234.84μg/L。
3.分别以最低定量限和4倍最低定量限为添加浓度对生姜样品进行了两个水平的添加回收率实验,方法的回收率范围为53.6~132.6 %(其中回收率在70 %~120 %的占94.9 %),相对标准偏差范围为0.4 %~25 %。
该方法操作简便,灵敏度、准确度和精密度均符合农药多残留检测技术要求,适用于生姜中215种农药多残留的快速测定。
Pesticides are indispensable material in agricultural production, that used to control or prevention of diseases, insects and weeds. The extensive use of pesticides plays an important role in the increase of food production. However , with the development of science and technology , the species and the number of chemical pesticides are increasing. Because of the long-term large-scale use and abuse of pesticides, the hazards they have brought along with them to food safety and human health have increasingly become the focus of world attention. Ginger is not only condiment and food in our diet , but also one of important export vegetables. During the planting period the ginger is challenged by various plant diseases, insect pests and weeds, affect the yield of the ginger. Pesticides are routinely administered in order to maximise ginger. Together with other types of pesticides in soil, ginger can be contaminated by a variety of pesticides. This situation has let to many countries increased the detection items of pesticide residues in the import/export of ginger, established more and more stringent standards and MRL, which shows a decreasing trend over recent years. It’s frequent occurrenced, that China's exports were returned by the importing country . This paper studied extraction, purification and LC-MS/MS detection conditions of pesticide residues in ginger, and establishing the method for determination of 215 pesticide residues in ginger, which cleaning-up by SPE and determined by the high- performance liquid chromatography-tandem mass spectrometry.
The main results were as follows:
1. We optimized the extract solvent, extract method, clean up method, then established a method, that homogeneous extracted by acetonitrile (containing 1% acetate acid),cleaned-up by Waters Sep-Pak Vac, for extract and clean up pesticide residues in ginger.
2. We established the LC-MS/MS detection method for 215 pesticides. 203 pesticides correlation coefficient above 0.99, accounting for 94 percent of the detected pesticides. The limits of detection and the limits of quantification were 0.01~70.45μg/L, 0.04~234.84μg/L respectively.
3. The recovery was conducted at two spiked levels which is the LOQ concentration and 4 times of LOQ concentration, the validation results were as follows: the overall recoveries were from 53.6 % to 132.6 % (94.9 % of the recoveries were from 70 % to 120 %), with the relative standard deviations (RSDS) of 0.4 %-25 %.
The method is simple. It’s sensitivity, accuracy and precision meet the requirements of the multiple pestiside residues. This method is applicable to rapid determination 215 pesticide residues in ginger.
主要研究结果如下:
1.对实验的提取溶剂、提取方法、净化方式进行了研究,建立了采用1%的醋酸乙腈均质提取、Waters Sep-Pak Vac固相萃取柱净化的方法从生姜中提取净化多种农药残留。
2.液相色谱-串联质谱检测方面,建立了215种农药残留液相色谱-串联质谱检测方法。结果表明,215种农药在相应的质量浓度范围内,各农药的响应值与其质量浓度均成良好的线性范围,215种农药线性相关系数大于0.99的有203个,占总数的94 %。215种农药的最小检出限为0.01~70.45μg/L;最低定量限范围为0.04~234.84μg/L。
3.分别以最低定量限和4倍最低定量限为添加浓度对生姜样品进行了两个水平的添加回收率实验,方法的回收率范围为53.6~132.6 %(其中回收率在70 %~120 %的占94.9 %),相对标准偏差范围为0.4 %~25 %。
该方法操作简便,灵敏度、准确度和精密度均符合农药多残留检测技术要求,适用于生姜中215种农药多残留的快速测定。
Pesticides are indispensable material in agricultural production, that used to control or prevention of diseases, insects and weeds. The extensive use of pesticides plays an important role in the increase of food production. However , with the development of science and technology , the species and the number of chemical pesticides are increasing. Because of the long-term large-scale use and abuse of pesticides, the hazards they have brought along with them to food safety and human health have increasingly become the focus of world attention. Ginger is not only condiment and food in our diet , but also one of important export vegetables. During the planting period the ginger is challenged by various plant diseases, insect pests and weeds, affect the yield of the ginger. Pesticides are routinely administered in order to maximise ginger. Together with other types of pesticides in soil, ginger can be contaminated by a variety of pesticides. This situation has let to many countries increased the detection items of pesticide residues in the import/export of ginger, established more and more stringent standards and MRL, which shows a decreasing trend over recent years. It’s frequent occurrenced, that China's exports were returned by the importing country . This paper studied extraction, purification and LC-MS/MS detection conditions of pesticide residues in ginger, and establishing the method for determination of 215 pesticide residues in ginger, which cleaning-up by SPE and determined by the high- performance liquid chromatography-tandem mass spectrometry.
The main results were as follows:
1. We optimized the extract solvent, extract method, clean up method, then established a method, that homogeneous extracted by acetonitrile (containing 1% acetate acid),cleaned-up by Waters Sep-Pak Vac, for extract and clean up pesticide residues in ginger.
2. We established the LC-MS/MS detection method for 215 pesticides. 203 pesticides correlation coefficient above 0.99, accounting for 94 percent of the detected pesticides. The limits of detection and the limits of quantification were 0.01~70.45μg/L, 0.04~234.84μg/L respectively.
3. The recovery was conducted at two spiked levels which is the LOQ concentration and 4 times of LOQ concentration, the validation results were as follows: the overall recoveries were from 53.6 % to 132.6 % (94.9 % of the recoveries were from 70 % to 120 %), with the relative standard deviations (RSDS) of 0.4 %-25 %.
The method is simple. It’s sensitivity, accuracy and precision meet the requirements of the multiple pestiside residues. This method is applicable to rapid determination 215 pesticide residues in ginger.
引文
曾小星,万益群,谢明勇.微波辅助萃取-气相色谱法测定茶叶中多种有机氯和拟除虫菊酯农药残留[J].食品科学, 2008, 29(11): 562-566.
陈青,刘志敏.超临界流体色谱的研究进展[J].分析化学, 2004, 32(8): 1104-1109.
程定玺,赵亚鹏,高曼.荧光法快速检测有机磷农药残留总量[J].分析试验室, 2010, 29(2): 45-48.
戴华,李拥军,张莹.稻谷中吡虫啉农药残留量的固相萃取高效液相色谱测定[J].分析测试学报, 2002, 21(1): 70-72.
高颖,赵红燕,安伟娟,李娜,李春飞.固相萃取-高效液相色谱法检测大米中咪唑乙烟酸和米草酸[J].现代测量与实验室管理, 2008(5):7-9.
归秀娥.我国农产品出口受阻于国外绿色壁垒的原因与对策[J].西安财经学院学报, 2010, 23(1): 91-94.
洪月玲,钟红舰,董小海.LC - MS/MS法测定水果、蔬菜中多菌灵残留的研究[J].河南预防医学杂志, 2008, 29(1): 19-21.
侯如燕,蔡荟梅,张正竹,宛晓春.液相色谱法检测水果蔬菜中的烟碱类农药残留[J].分析实验室, 2010, 29(2): 59-63.
胡贝贞,宋伟华,谢丽萍,邵铁锋.气相色谱-负化学离子源质谱法测定含硫蔬菜中的14种农药残留[J].色谱, 2008, 26(5): 608-612.
胡彦学,杨秀敏,张美月,李卫宁,王春,王志.固相微萃取—高效液相色谱联用测定番茄中氨基甲酸酯类农药残留[J].中国食品学报, 2008, 8(6): 155-160.
黄琼辉.国内外农药残留检测技术研究进展和发展方向[J].福建农业学报, 2008, 23(2): 218-222.
李欢欣,赵春杰.超临界流体萃取法净化熟地中有机氯农药的研究[J].中国医院药学杂志, 2008, 28(8): 607-611.
李文秀,徐可欣,汪嚥，雷震霖，张振厚.蔬菜农药残留检测的红外光谱法研究[J].光谱学与光谱分析, 2004, 24(10): 1202-1204.
李昕,孔祥虹,刘勇,张静.UPLC法测定浓缩苹果汁中阿维菌素残留量[J]. 分析试验室, 2009, 28(11): 74-76.
林振宇,黄露,陈国南.毛细管电泳和毛细管电色谱技术在农药残留检测中的应用[J].色谱, 2009, 27(1): 9-18.
刘少军,陈巍,梁学亮.出口生姜的农药选择和使用[J].中国检验检疫,2008,(6) :30.
刘祥国,于洪意,李旭宁.药物残留检测的样品前处理技术新进展(上)[J]. 畜产品安全, 2007, (6): 33-35.
罗俊霞,符建伟,李德瑜,杜凤山,赵建波,郭华婷.微波处理-气相色谱法测定蒜苔中多种有机氯、拟除虫菊酯类农药残留[J].分析试验室, 2008, 27(增刊): 172-175.
潘玉香,董静,孙军,张靖,朱莉萍.气相色谱法测定复杂基质蔬菜中11种农药的残留量[J].理化检验-化学分册, 2009, 45(7): 852-854.
裴道国,崔淑华,王雄,王莲,惠小敏.免疫亲合柱净化-气相色谱质谱法测定花生和大蒜中乙草胺残留量[J].中国食品卫生杂志, 2008, 20 (5): 418-420.
沈旭,陈晓辉,果德安,张舒婷,毕开顺.中空纤维液相微萃取-气相色谱法测定白芍中20种农药残留[J].药物分析杂志, 2009, 29(10): 1745- 1748.
宋文华,刘芳,丁峰,高敏苓,王国峰.液相色谱-质谱联用法快速检测蔬菜水果中70种农药多残留分析的研究[J].南开大学学报, 2008, 41 (2): 35-41.
孙福生,董杰.基质固相分散-反相液相色谱法测定蔬菜中二甲戊乐灵农药残留[J].分析试验室, 2010, 29(2): 69-72.
汤凯洁,顾小红,陶冠军,秦芳,汤坚,夏咏梅.分子印迹固相萃-液相色谱质谱联用对4种磺酰脲类除草剂残留的测定[J].分析测试学报, 2009, 28(12): 1401-1404.
王建,贾斌,张伟国.气相色谱-三重四极质谱对复杂基质蔬菜(洋葱、茴香)中12种农药残留量的同时测定[J].分析测试学报, 2008, 27(增刊): 177-179.
王建华,张艺兵,汤志旭,刘心同.微波处理-气相色谱法测定含硫蔬菜中的多类农药残留[J].分析测试学报, 2005, 24(1): 100-102.
王静,金芬,邵华,杨锚.农药多残留检测样品前处理技术研究进展[J].农业质量标准, 2007, 1: 28-31.
王连珠,杨明智,王瑞龙,郑俊超,刘溢娜.气相色谱-质谱法测定生姜中丙炔氟草胺残留量[J].食品科学, 2006, 27(10): 461-463.
王文珺,刘兴春,李季.免疫分析在农药残留检测中的应用和发展[J].中国生态农业学报, 2007, 15(6): 195-199.
王勇,周宏琛,闫秋成.高效液相色谱法测定大蒜中吡虫啉残留[J].济宁师范专科学校学报, 2006, 27(3): 16-17.
王玉田,刘蕊.监测氨基甲酸酯类农药的光纤荧光光谱仪的研究[J].传感技术学报, 2003,(3): 318-320.
吴赛苏,丁小交.薄层色谱法检测久效磷农药的残留量[J].广东化工, 2009, 36(7): 228-229.
杨惠琴,郭德华,李波,朱坚,韩丽,王敏,邓晓军,盛永刚.凝胶色谱串联质谱法检测植物性产品中75种农药残留[J].中国卫生检验杂志, 2007, l7(8): 1355-1358.
杨长志,张晓华,康庆贺,韩广源.高效液相色谱法测定大米中抑虫肼的残留量[J].化学工程师, 2006, 134: 27-29.
应剑波,谢伟宏,程建波,金立方,郑强.微波萃取-GPC净化-GC/ MS法检验血中氨基甲酸酯和沙蚕毒素类农药[J].质谱学报, 2009, 30(1): 47 -50.
张国华,赖卫华,金晶,盛志超.免疫亲合色谱的原理及其在食品安全检测中的应用[J].食品科学, 2007, 28(1): 577-581.
张齐家,孙文军.串联质谱及液质联用技术在药物分析研究中的应用[J].中医药学报, 2009, 37(6): 111-113.
张琦,李达.气相色谱法测定姜中毒死蜱农药的残留量[J].化学工程师, 2007, 143(8): 21-23.
赵海香,袁光耀,邱月明,汪丽萍,周志强.加速溶剂萃取技术(ASE)在农药残留分析中的应用[J].农药, 2006, 45(1): 15-17.
支建梁,牟仁祥,陈铭学,朱智伟.柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂[J].色谱, 2008, 26(1): 93-97.
朱将伟.农产品中农药残留检测技术及监管措施概述[J].饲料工业, 2010, 31 (1): 36-39.
Antignaca Jean-Philippe, Waschb Katia de, Monteaua Fabrice, Brabanderb Hubert De, Andrea Franc?ois, Bizeca Bruno Le. The ion suppression phenomenon in liquid chromatography-mass spectrometry and its consequences in the field of residue analysis[J]. Analytica Chimica Acta , 2005, 529: 129-136.
Armenta Sergio, Quintas Guillermo, Garrigues Salvador, Guardia Miguel de la. A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos[J].Talanta , 2005, 67: 634–639.
Arthur C L, Pawliszyn J. Solid phase-with thermal desorption using fused silica optical fibers[J]. Analytical Chemistry, 1990, 62: 2145-2148. Benijts Tom, Dams Riet, Lambert Willy, Leenheer AndréDe. Countering matrix effects in environmental liquid Chromatography -electrospray ionization tandem mass spectrometry water analysis for endocrine disrupting chemicals[J]. Journal of Chromatography A, 2004, 1029: 153- 159.
Barker S A, Long A R, Short C R. Isolation of drug residues from tissues by solid phase dispersion[J]. Journal of Chromatography A, 1989, 475: 353 -361.
Bienvenida Gilbert-Lópeza, Juan F. García-Reyesa, Milagros Mezcuab, Natividad Ramos-Martosa, Amadeo R.Fernández-Albab, Antonio Molina- Díaza. Multi-residue determination of pesticides in fruit-based soft drinks by fast liquid chromatography time-of-flight mass spectrometry[J]. Talanta, 2010, 81: 1310-1321.
BlazkováMartina, Micková-HolubováBarbora, Rauch Pavel, Fukal Ladislav.Immunochromatographic colloidal carbon-based assay for detection of methiocarb in surface water [J ]. Biosensors and Bioelectronics, 2009, 25: 753–758.
Bordier C. Phase separation of integralmembrane proteins in TritonX-114 solution [J ]. Biol Chem , 1981, 256 (8) : 1604 - 1607.
Carabias-Martinez R., Rodriguez-Gonzalo E., Miranda-Cruz E., Dominguez-Alvarez J., Hernandez-Mendez J..Comparison of a non- aqueous capillary electrophoresis method with high performance liquid chromatography for the determination of herbicides and metabolites in water samples[J]. Journal of Chromatography A, 2006, 1122: 194-201.
Chen Zilei, Zhang Hong, Liu Bing, Yang Guosheng, Aboul-Enein Hassan Y., Wang Wenbo, Ding Ruiyan, Du Hongxia, Li Huidong. Determination of Herbicide Residues in Garlic by GC-MS [J]. Chromatographia, 2007, 66: 887-891.
Chuang Jane C., Van Emonb Jeanette M., Jones Randy, Durnford Joyce , Lordo Robert A.. Development and application of immunoaffinity column chromatography for atrazine in complex sample media [J]. Analytica Chimica Acta, 2007, 583: 32–39.
Dagnac Thierry, Garcia-Chao Maria, Pulleiro Paula, Garcia-Jares Carmen, Llompart Maria. Dispersive solid-phase extraction followed by liquid chromatography–tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk[J].Journal of Chromatography A, 2009, 1216: 3702–3709.
Dasgupta Soma, Banerjee Kaushik, Patil Sangram H., Ghaste Manoj, Dhumal K.N.,Adsulea Pandurang G.. Optimization of two-dimensional gas chromatography time-of-flight mass spectrometry for separation and estimation of the residues of 160 pesticides and 25 persistent organic pollutants in grape and wine[J].Journal of Chromatography A, 2010, 1217: 3881–3889.
Derouiche A., Driss M.R., Morizur J.P., Taphanel M.H.. Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in water by headspace solid-phase microextraction with gas chromatography- tandem mass spectrometry[J].Journal of Chromatography A, 2007, 1138: 231-243. Economou Anastasios,Botitsi Helen,Antoniou Spyros,Tsipi Despina.
Determination of multi-class pesticides in wines by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2009, 1216: 5856-5867.
Imma Ferrer , Michael Thurmanb E. . Multi-residue method for the analysis of 101 pesticides and their degradates in food and water samples by liquid chromatography/time-of-flight mass spectrometry[J]. Journal of Chromatography A, 2007, 1175: 24-37.
Ganzler Katalin, SalgóAndrás, ValkóKlára. Microwave extraction : A novel sample preparation method for chromatography[J]. Journal of Chromatography A, 1986, 371: 299-306.
García-Galán M. Jesús , Díaz-Cruz M. Silvia, BarcelóDamià. Determination of triazines and their metabolites in environmental samples using molecularly imprinted polymer extraction, pressurized liquid extraction and LC–tandem mass spectrometry[J]. Journal of Hydrology, 2010 ,383: 30-38.
Guidance document on residue analytical methods,SANCO/825/00 rev. 717/03/2004
Guardia-Rubio M., Marchal-Lopez R.M., Ayora-Canada M.J., Ruiz- Medina A.. Determination of pesticides in olives by gas chromatography using different detection systems[J]. Journal of Chromatography A, 2007, 1145: 195-203.
Guler G.O., Cakmak Y.S., Dagli Z. , Aktumsek A. , Ozparlak H.. Organochlorine pesticide residues in wheat from Konya region, Turkey [J]. Food and Chemical Toxicology, 2010, 48: 1218-1221. GUO Qing, LV Xia, TAN Li, YU Bo-Yang. Simultaneous Determination of 26 Pesticide Residues in 5 Chinese Medicinal Materials Using Solid- phase Extraction and GC-ECD Method[J]. Chinese Journal of Natural Medicines , 2009, 7(3): 210-216.
Hernandez F., Pozo O.J., Sancho J.V., Bijlsma L., Barreda M., Pitarch E.. Multiresidue liquid chromatography tandem mass spectrometry determination of 52 non gas chromatography-amenable pesticides and metabolites in different food commodities[J].Journal of Chromatography A , 2006, 1109: 242-252.
Jame A.T., Martin A.J.. Gas-liquid partition chromatography; the separation and micro-estimation of volatile fatty acids from formic acid to dodecanoic acid[J]. The Biochemical journal, 1952, 50(5): 679-690.
Jeannot M. A., Cantwell F. F.. Solvent microextraction into a single drop[J]. Analytical Chemistry, 1996, 68: 2236-2240.
Jia GuiFang, Lv ChunGuang, Zhu WenTao, Qiu Jing, Wang XinQuan, Zhou ZhiQiang. Applicability of cloud point extraction coupled with microwave-assisted back-extraction to the determination of organophosphorous pesticides in human urine by gas chromatography with flame photometry detection[J]. Journal of Hazardous Materials, 2008, 159: 300-305.
Juan-García Ana, Font Guillermina, Juan Cristina, PicóYolanda. Pressurised liquid extraction and capillary electrophoresis–mass spectrometry for the analysis of pesticide residues in fruits from Valencian markets, Spain[J]. Food Chemistry, 2010, 120: 1242-1249.
Knezevic Zorka, Serdar Maja. Screening of fresh fruit and vegetables for pesticide residues on Croatian market[J]. Food Control, 2009, 20: 419-422.
Kruve Anneli, Kunnapas Allan, Herodes Koit , Leito Ivo. Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2008, 1187: 58-66.
Lee Jeong-Min , Park Jin-Won, Jang Gi-Chul, Hwang Keon-Joong. Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry[J]. Journal of Chromatography A, 2008, 1187: 25-33.
Lesueur C., Knittl P. , Gartner M., Mentler A., Fuerhacker M.. Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuECheRS method[J].Food Control, 2008 , 19: 906- 914.
Marín JoséM., Gracia-Lor Emma, Sancho Juan V., López Francisco J., Hernández Félix.Application of ultra-high-pressure liquid chromatography-tandem mass spectrometry to the determination of multi-class pesticides in environmental and wastewater samples Study of matrix effects[J]. Journal of Chromatography A, 2009, 1216: 1410-1420.
Martfnez Galera M., Martfnez Vidal J.L., Garrido Frenich A., Gil Garcia M.D. . Determination of cypermethrin, fenvalerate and cis- and trans- permethrin in soil and groundwater by high-performance liquid chromatography using partial least-squares regression [J]. Journal of Chromatography A, 1996, 727: 39-46.
Miura Junichiro, Ishii Hideki, Watanabe Hiroto. Extraction and separation of nickel chelates of 1-(2-thiazolylazo)-2- naphthol in nonionic surfactant solution[J]. Bunseki Kagaku , 1976, 25(11): 808-809.
Nam Ki-Souk , Jerry W. King. Coupled SFE/SFC/GC for the trace analysis of pesticide residues in fatty food samples[J].Journal of High Resolution Chromatography, 1994, 17: 577-582.
Nguyen Thanh Dong, Lee Myoung Hee, Lee Gae Ho. Rapid determination of95 pesticides in soybean oil using liquid-liquid extraction followed by centrifugation, freezing and dispersive solid phase extraction as cleanup steps and gas chromatography with mass spectrometric detection[J]. Microchemical Journal, 2010, 95: 113-119.
Nguyen Thanh Dong, Lee Kyung Jun, Lee Myoung Hee , Lee Gae Ho. A multiresidue method for the determination 234 pesticides in Korean herbs using gas chromatography mass spectrometry[J]. Microchemical Journal, 2010, 95: 43-49.
Pang Guo-Fang, Cao Yan-Zhong, Zhang Jin-Jie, Fan Chun-Lin, Liu Yong- Ming, Li Xue-Min. Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography- mass spectrometry and liquid chromatography-tandem mass spectrometry [J]. Journal of Chromatography A, 2006,1125: 1-30.
Pedersen Bjergaard S, Rasmussen K E. . Liquid-liquid-liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis[J]. Analytical Chemistry, 1999, 71(14): 2650- 2656.
Pizzutti Ionara R., Kok Andre de, Zanella Renato, Adaime Martha B., Hiemstra Maurice, Wickert Cristine, Prestes Osmar D.. Method validation for the analysis of 169 pesticides in soya grain, without clean up , by liquid chromatography–tandem mass spectrometry using positive and negative electrospray ionization[J]. Journal of Chromatography A, 2007, 1142: 123- 136.
Queiroz A A A, Ferraz H G, Abraham G A, et al. Development of new hydroactive dressings based on chitosan membranes:Characterization and in vivo behavior[J]. Journal of Biomedical Materials Research Part A,2003, 64A(1): 147-154.
Rezic I., Horvat A.J.M., Babic S., Kastelan-Macan M.. Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography[J]. Ultrasonics Sonochemistry, 2005, 12: 477-481.
Richter B. E. , Ezzell J. L. , Felix D , Roberts K. A. , Later D. W.. An accelerated solvent extraction system for the rapid preparation of environmental organic compounds in soil[J]. American Laboratory , 1995, 27 (4) : 24-28.
Ridgway Kathy, Lalljie Sam P.D., Smith Roger M.. Sample preparationtechniques for the determination of trace residues and contaminants in foods[J]. Journal of Chromatography A, 2007, 1153: 36-53.
Rissato Sandra R., Galhianea Mario S., Knollb Fatima R.N., Apon Bernhard M.. Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with electron-capture and mass spectrometry detection[J]. Journal of Chromatography A, 2004, 1048: 153-159.
Sanusi Astrid, Guillet Valérie, Montury Michel. Advanced method using microwaves and solid-phase microextraction coupled with gas chromatography-mass spectrometry for the determination of pyrethroid residues in strawberries[J]. Journal of Chromatography A, 2004, 1046: 35-46.
Smalling Kelly L., Kuivila Kathryn M.. Multi-residue method for the analysis of 85 current-use and legacy pesticides in bed and suspended sediments [J].Journal of Chromatography A, 2008, 1210: 8-18.
Petr Suchan, PulkrabováJana, Haj?lováJ ana, Kocourek Vladimir. Pressurized liquid extraction in determination of polychlorinated biphenyls and organochlorine pesticides in fish samples[J]. Analytica Chimica Acta, 2004, 520: 193-200.
Valera Enrique, Ramón-Azcón Javier, Barranco Alejandro, Alfaro Bego?a, Francisco Sánchez-Baeza, Marco M.-P., Rodríguezángel. Determination of atrazine residues in red wine samples. A conductimetric solution[J]. Food Chemistry, 2010, 122: 888-894.
Van De Steene Jet C., Mortier Kjell A., Lambert Willy E.. Tackling matrix effects during development of a liquid Chromatographic-electrospray ionisation tandem mass spectrometric analysis of nine basic pharmaceuticals in aqueous environmental samples[J]. Journal of Chromatography A, 2006, 1123: 71-81.
Van De Steene Jet C. , Lambert Willy E.. Comparison of Matrix Effects in HPLC-MS/MS and UPLC-MS/MS Analysis of Nine Basic
Pharmaceuticals in Surface Waters[J]. Am Soc Mass Spectrom , 2008, 19: 713-718.
Wang Jian Hua, Xu Qiang, Jiao Kui. Supercritical fluid extraction and off-line clean-up for the analysis of organochlorine pesticide residues in garlic[J].Journal of Chromatography A, 1998, 818: 138-143.
Wang Yuanfeng , Du Ran. Simultaneous extraction of trace organophosphorous pesticides from plasma sample by automated solid phase extraction and determination by gas chromatography coupled with pulsed flame photometric detector[J]. Forensic Science International , 2010, 198: 70-73.
Watanabe H, Tanaka H. A nonionic surfactant as a new solvent for liquid- liquid extraction of Zinc ( II) with 1-(2-pyridylazo)-2-naphthol [J ]. Talanta, 1978, 25 (4): 585-589.
Wenclawiak B., Otterbach A.. Carbon-based quantitation of pyrethrins by supercritical-fluid chromatography[J ]. Biochem. Biophys. Methods , 2000, 43: 197-207.
Xie Shunping, Paaua Man Chin, Li Cheuk Fai, Xiao Dan, Choia Martin M.F.. Separation and preconcentration of persistent organic pollutants by cloud point extraction[J]. Journal of Chromatography A, 2010, 1217 : 2306- 2317.
Xu Dun-ming,Yang Fang, Lu Sheng-yu, Jin-Chang. Determination of indoxacarb residue in foodstuffs of plant and animal origin by GC-ECD and LC-MS/MS[J]. Agricultural Sciences in China, 2008, 7(10): 1228- 1234.
Yang Ruiqiang, Wang Yawei, Li An, Zhang Qinghua, Jing Chuanyong, Wang Thanh, Wang Pu, Li Yingming, Jiang Guibin. Organochlorine pesticides and PCBs in fish from lakes of the Tibetan Plateau and the implications[J]. Environmental Pollution , 2010, 158: 2310-2316.
You Jing, Wang Dongli, Lydy Michael J.. Determination of pyrethroid insecticides in sediment by gas chromatography-Ion trap tandem mass spectrometry[J].Talanta, 2010, 81: 136-141.
Zhang Hong ,Chen Zilei ,Yang Guosheng ,Wang Wenzheng ,Li Xiuqing , Li Ruiju ,Wu Yuanjuan. Microwave pretreatment and gas chromatography- mass spectrometry determination of herbicide residues in onion[J].Food Chemistry, 2008, 108: 322–328.
Zhao Limian, Lee Hian Kee. Application of static liquid-phase microextraction to the analysis of organochlorine pesticides in water[J]. Journal of Chromatography A, 2001, 919: 381-388.
Zhou Jihai, Chen Jiandong, Cheng Yanhong, Li Daming, Hu Feng, Li Huixin. Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction[J].Talanta, 2009, 79: 189-193.
陈青,刘志敏.超临界流体色谱的研究进展[J].分析化学, 2004, 32(8): 1104-1109.
程定玺,赵亚鹏,高曼.荧光法快速检测有机磷农药残留总量[J].分析试验室, 2010, 29(2): 45-48.
戴华,李拥军,张莹.稻谷中吡虫啉农药残留量的固相萃取高效液相色谱测定[J].分析测试学报, 2002, 21(1): 70-72.
高颖,赵红燕,安伟娟,李娜,李春飞.固相萃取-高效液相色谱法检测大米中咪唑乙烟酸和米草酸[J].现代测量与实验室管理, 2008(5):7-9.
归秀娥.我国农产品出口受阻于国外绿色壁垒的原因与对策[J].西安财经学院学报, 2010, 23(1): 91-94.
洪月玲,钟红舰,董小海.LC - MS/MS法测定水果、蔬菜中多菌灵残留的研究[J].河南预防医学杂志, 2008, 29(1): 19-21.
侯如燕,蔡荟梅,张正竹,宛晓春.液相色谱法检测水果蔬菜中的烟碱类农药残留[J].分析实验室, 2010, 29(2): 59-63.
胡贝贞,宋伟华,谢丽萍,邵铁锋.气相色谱-负化学离子源质谱法测定含硫蔬菜中的14种农药残留[J].色谱, 2008, 26(5): 608-612.
胡彦学,杨秀敏,张美月,李卫宁,王春,王志.固相微萃取—高效液相色谱联用测定番茄中氨基甲酸酯类农药残留[J].中国食品学报, 2008, 8(6): 155-160.
黄琼辉.国内外农药残留检测技术研究进展和发展方向[J].福建农业学报, 2008, 23(2): 218-222.
李欢欣,赵春杰.超临界流体萃取法净化熟地中有机氯农药的研究[J].中国医院药学杂志, 2008, 28(8): 607-611.
李文秀,徐可欣,汪嚥，雷震霖，张振厚.蔬菜农药残留检测的红外光谱法研究[J].光谱学与光谱分析, 2004, 24(10): 1202-1204.
李昕,孔祥虹,刘勇,张静.UPLC法测定浓缩苹果汁中阿维菌素残留量[J]. 分析试验室, 2009, 28(11): 74-76.
林振宇,黄露,陈国南.毛细管电泳和毛细管电色谱技术在农药残留检测中的应用[J].色谱, 2009, 27(1): 9-18.
刘少军,陈巍,梁学亮.出口生姜的农药选择和使用[J].中国检验检疫,2008,(6) :30.
刘祥国,于洪意,李旭宁.药物残留检测的样品前处理技术新进展(上)[J]. 畜产品安全, 2007, (6): 33-35.
罗俊霞,符建伟,李德瑜,杜凤山,赵建波,郭华婷.微波处理-气相色谱法测定蒜苔中多种有机氯、拟除虫菊酯类农药残留[J].分析试验室, 2008, 27(增刊): 172-175.
潘玉香,董静,孙军,张靖,朱莉萍.气相色谱法测定复杂基质蔬菜中11种农药的残留量[J].理化检验-化学分册, 2009, 45(7): 852-854.
裴道国,崔淑华,王雄,王莲,惠小敏.免疫亲合柱净化-气相色谱质谱法测定花生和大蒜中乙草胺残留量[J].中国食品卫生杂志, 2008, 20 (5): 418-420.
沈旭,陈晓辉,果德安,张舒婷,毕开顺.中空纤维液相微萃取-气相色谱法测定白芍中20种农药残留[J].药物分析杂志, 2009, 29(10): 1745- 1748.
宋文华,刘芳,丁峰,高敏苓,王国峰.液相色谱-质谱联用法快速检测蔬菜水果中70种农药多残留分析的研究[J].南开大学学报, 2008, 41 (2): 35-41.
孙福生,董杰.基质固相分散-反相液相色谱法测定蔬菜中二甲戊乐灵农药残留[J].分析试验室, 2010, 29(2): 69-72.
汤凯洁,顾小红,陶冠军,秦芳,汤坚,夏咏梅.分子印迹固相萃-液相色谱质谱联用对4种磺酰脲类除草剂残留的测定[J].分析测试学报, 2009, 28(12): 1401-1404.
王建,贾斌,张伟国.气相色谱-三重四极质谱对复杂基质蔬菜(洋葱、茴香)中12种农药残留量的同时测定[J].分析测试学报, 2008, 27(增刊): 177-179.
王建华,张艺兵,汤志旭,刘心同.微波处理-气相色谱法测定含硫蔬菜中的多类农药残留[J].分析测试学报, 2005, 24(1): 100-102.
王静,金芬,邵华,杨锚.农药多残留检测样品前处理技术研究进展[J].农业质量标准, 2007, 1: 28-31.
王连珠,杨明智,王瑞龙,郑俊超,刘溢娜.气相色谱-质谱法测定生姜中丙炔氟草胺残留量[J].食品科学, 2006, 27(10): 461-463.
王文珺,刘兴春,李季.免疫分析在农药残留检测中的应用和发展[J].中国生态农业学报, 2007, 15(6): 195-199.
王勇,周宏琛,闫秋成.高效液相色谱法测定大蒜中吡虫啉残留[J].济宁师范专科学校学报, 2006, 27(3): 16-17.
王玉田,刘蕊.监测氨基甲酸酯类农药的光纤荧光光谱仪的研究[J].传感技术学报, 2003,(3): 318-320.
吴赛苏,丁小交.薄层色谱法检测久效磷农药的残留量[J].广东化工, 2009, 36(7): 228-229.
杨惠琴,郭德华,李波,朱坚,韩丽,王敏,邓晓军,盛永刚.凝胶色谱串联质谱法检测植物性产品中75种农药残留[J].中国卫生检验杂志, 2007, l7(8): 1355-1358.
杨长志,张晓华,康庆贺,韩广源.高效液相色谱法测定大米中抑虫肼的残留量[J].化学工程师, 2006, 134: 27-29.
应剑波,谢伟宏,程建波,金立方,郑强.微波萃取-GPC净化-GC/ MS法检验血中氨基甲酸酯和沙蚕毒素类农药[J].质谱学报, 2009, 30(1): 47 -50.
张国华,赖卫华,金晶,盛志超.免疫亲合色谱的原理及其在食品安全检测中的应用[J].食品科学, 2007, 28(1): 577-581.
张齐家,孙文军.串联质谱及液质联用技术在药物分析研究中的应用[J].中医药学报, 2009, 37(6): 111-113.
张琦,李达.气相色谱法测定姜中毒死蜱农药的残留量[J].化学工程师, 2007, 143(8): 21-23.
赵海香,袁光耀,邱月明,汪丽萍,周志强.加速溶剂萃取技术(ASE)在农药残留分析中的应用[J].农药, 2006, 45(1): 15-17.
支建梁,牟仁祥,陈铭学,朱智伟.柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂[J].色谱, 2008, 26(1): 93-97.
朱将伟.农产品中农药残留检测技术及监管措施概述[J].饲料工业, 2010, 31 (1): 36-39.
Antignaca Jean-Philippe, Waschb Katia de, Monteaua Fabrice, Brabanderb Hubert De, Andrea Franc?ois, Bizeca Bruno Le. The ion suppression phenomenon in liquid chromatography-mass spectrometry and its consequences in the field of residue analysis[J]. Analytica Chimica Acta , 2005, 529: 129-136.
Armenta Sergio, Quintas Guillermo, Garrigues Salvador, Guardia Miguel de la. A validated and fast procedure for FTIR determination of Cypermethrin and Chlorpyrifos[J].Talanta , 2005, 67: 634–639.
Arthur C L, Pawliszyn J. Solid phase-with thermal desorption using fused silica optical fibers[J]. Analytical Chemistry, 1990, 62: 2145-2148. Benijts Tom, Dams Riet, Lambert Willy, Leenheer AndréDe. Countering matrix effects in environmental liquid Chromatography -electrospray ionization tandem mass spectrometry water analysis for endocrine disrupting chemicals[J]. Journal of Chromatography A, 2004, 1029: 153- 159.
Barker S A, Long A R, Short C R. Isolation of drug residues from tissues by solid phase dispersion[J]. Journal of Chromatography A, 1989, 475: 353 -361.
Bienvenida Gilbert-Lópeza, Juan F. García-Reyesa, Milagros Mezcuab, Natividad Ramos-Martosa, Amadeo R.Fernández-Albab, Antonio Molina- Díaza. Multi-residue determination of pesticides in fruit-based soft drinks by fast liquid chromatography time-of-flight mass spectrometry[J]. Talanta, 2010, 81: 1310-1321.
BlazkováMartina, Micková-HolubováBarbora, Rauch Pavel, Fukal Ladislav.Immunochromatographic colloidal carbon-based assay for detection of methiocarb in surface water [J ]. Biosensors and Bioelectronics, 2009, 25: 753–758.
Bordier C. Phase separation of integralmembrane proteins in TritonX-114 solution [J ]. Biol Chem , 1981, 256 (8) : 1604 - 1607.
Carabias-Martinez R., Rodriguez-Gonzalo E., Miranda-Cruz E., Dominguez-Alvarez J., Hernandez-Mendez J..Comparison of a non- aqueous capillary electrophoresis method with high performance liquid chromatography for the determination of herbicides and metabolites in water samples[J]. Journal of Chromatography A, 2006, 1122: 194-201.
Chen Zilei, Zhang Hong, Liu Bing, Yang Guosheng, Aboul-Enein Hassan Y., Wang Wenbo, Ding Ruiyan, Du Hongxia, Li Huidong. Determination of Herbicide Residues in Garlic by GC-MS [J]. Chromatographia, 2007, 66: 887-891.
Chuang Jane C., Van Emonb Jeanette M., Jones Randy, Durnford Joyce , Lordo Robert A.. Development and application of immunoaffinity column chromatography for atrazine in complex sample media [J]. Analytica Chimica Acta, 2007, 583: 32–39.
Dagnac Thierry, Garcia-Chao Maria, Pulleiro Paula, Garcia-Jares Carmen, Llompart Maria. Dispersive solid-phase extraction followed by liquid chromatography–tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk[J].Journal of Chromatography A, 2009, 1216: 3702–3709.
Dasgupta Soma, Banerjee Kaushik, Patil Sangram H., Ghaste Manoj, Dhumal K.N.,Adsulea Pandurang G.. Optimization of two-dimensional gas chromatography time-of-flight mass spectrometry for separation and estimation of the residues of 160 pesticides and 25 persistent organic pollutants in grape and wine[J].Journal of Chromatography A, 2010, 1217: 3881–3889.
Derouiche A., Driss M.R., Morizur J.P., Taphanel M.H.. Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in water by headspace solid-phase microextraction with gas chromatography- tandem mass spectrometry[J].Journal of Chromatography A, 2007, 1138: 231-243. Economou Anastasios,Botitsi Helen,Antoniou Spyros,Tsipi Despina.
Determination of multi-class pesticides in wines by solid-phase extraction and liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2009, 1216: 5856-5867.
Imma Ferrer , Michael Thurmanb E. . Multi-residue method for the analysis of 101 pesticides and their degradates in food and water samples by liquid chromatography/time-of-flight mass spectrometry[J]. Journal of Chromatography A, 2007, 1175: 24-37.
Ganzler Katalin, SalgóAndrás, ValkóKlára. Microwave extraction : A novel sample preparation method for chromatography[J]. Journal of Chromatography A, 1986, 371: 299-306.
García-Galán M. Jesús , Díaz-Cruz M. Silvia, BarcelóDamià. Determination of triazines and their metabolites in environmental samples using molecularly imprinted polymer extraction, pressurized liquid extraction and LC–tandem mass spectrometry[J]. Journal of Hydrology, 2010 ,383: 30-38.
Guidance document on residue analytical methods,SANCO/825/00 rev. 717/03/2004
Guardia-Rubio M., Marchal-Lopez R.M., Ayora-Canada M.J., Ruiz- Medina A.. Determination of pesticides in olives by gas chromatography using different detection systems[J]. Journal of Chromatography A, 2007, 1145: 195-203.
Guler G.O., Cakmak Y.S., Dagli Z. , Aktumsek A. , Ozparlak H.. Organochlorine pesticide residues in wheat from Konya region, Turkey [J]. Food and Chemical Toxicology, 2010, 48: 1218-1221. GUO Qing, LV Xia, TAN Li, YU Bo-Yang. Simultaneous Determination of 26 Pesticide Residues in 5 Chinese Medicinal Materials Using Solid- phase Extraction and GC-ECD Method[J]. Chinese Journal of Natural Medicines , 2009, 7(3): 210-216.
Hernandez F., Pozo O.J., Sancho J.V., Bijlsma L., Barreda M., Pitarch E.. Multiresidue liquid chromatography tandem mass spectrometry determination of 52 non gas chromatography-amenable pesticides and metabolites in different food commodities[J].Journal of Chromatography A , 2006, 1109: 242-252.
Jame A.T., Martin A.J.. Gas-liquid partition chromatography; the separation and micro-estimation of volatile fatty acids from formic acid to dodecanoic acid[J]. The Biochemical journal, 1952, 50(5): 679-690.
Jeannot M. A., Cantwell F. F.. Solvent microextraction into a single drop[J]. Analytical Chemistry, 1996, 68: 2236-2240.
Jia GuiFang, Lv ChunGuang, Zhu WenTao, Qiu Jing, Wang XinQuan, Zhou ZhiQiang. Applicability of cloud point extraction coupled with microwave-assisted back-extraction to the determination of organophosphorous pesticides in human urine by gas chromatography with flame photometry detection[J]. Journal of Hazardous Materials, 2008, 159: 300-305.
Juan-García Ana, Font Guillermina, Juan Cristina, PicóYolanda. Pressurised liquid extraction and capillary electrophoresis–mass spectrometry for the analysis of pesticide residues in fruits from Valencian markets, Spain[J]. Food Chemistry, 2010, 120: 1242-1249.
Knezevic Zorka, Serdar Maja. Screening of fresh fruit and vegetables for pesticide residues on Croatian market[J]. Food Control, 2009, 20: 419-422.
Kruve Anneli, Kunnapas Allan, Herodes Koit , Leito Ivo. Matrix effects in pesticide multi-residue analysis by liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2008, 1187: 58-66.
Lee Jeong-Min , Park Jin-Won, Jang Gi-Chul, Hwang Keon-Joong. Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry[J]. Journal of Chromatography A, 2008, 1187: 25-33.
Lesueur C., Knittl P. , Gartner M., Mentler A., Fuerhacker M.. Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuECheRS method[J].Food Control, 2008 , 19: 906- 914.
Marín JoséM., Gracia-Lor Emma, Sancho Juan V., López Francisco J., Hernández Félix.Application of ultra-high-pressure liquid chromatography-tandem mass spectrometry to the determination of multi-class pesticides in environmental and wastewater samples Study of matrix effects[J]. Journal of Chromatography A, 2009, 1216: 1410-1420.
Martfnez Galera M., Martfnez Vidal J.L., Garrido Frenich A., Gil Garcia M.D. . Determination of cypermethrin, fenvalerate and cis- and trans- permethrin in soil and groundwater by high-performance liquid chromatography using partial least-squares regression [J]. Journal of Chromatography A, 1996, 727: 39-46.
Miura Junichiro, Ishii Hideki, Watanabe Hiroto. Extraction and separation of nickel chelates of 1-(2-thiazolylazo)-2- naphthol in nonionic surfactant solution[J]. Bunseki Kagaku , 1976, 25(11): 808-809.
Nam Ki-Souk , Jerry W. King. Coupled SFE/SFC/GC for the trace analysis of pesticide residues in fatty food samples[J].Journal of High Resolution Chromatography, 1994, 17: 577-582.
Nguyen Thanh Dong, Lee Myoung Hee, Lee Gae Ho. Rapid determination of95 pesticides in soybean oil using liquid-liquid extraction followed by centrifugation, freezing and dispersive solid phase extraction as cleanup steps and gas chromatography with mass spectrometric detection[J]. Microchemical Journal, 2010, 95: 113-119.
Nguyen Thanh Dong, Lee Kyung Jun, Lee Myoung Hee , Lee Gae Ho. A multiresidue method for the determination 234 pesticides in Korean herbs using gas chromatography mass spectrometry[J]. Microchemical Journal, 2010, 95: 43-49.
Pang Guo-Fang, Cao Yan-Zhong, Zhang Jin-Jie, Fan Chun-Lin, Liu Yong- Ming, Li Xue-Min. Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography- mass spectrometry and liquid chromatography-tandem mass spectrometry [J]. Journal of Chromatography A, 2006,1125: 1-30.
Pedersen Bjergaard S, Rasmussen K E. . Liquid-liquid-liquid microextraction for sample preparation of biological fluids prior to capillary electrophoresis[J]. Analytical Chemistry, 1999, 71(14): 2650- 2656.
Pizzutti Ionara R., Kok Andre de, Zanella Renato, Adaime Martha B., Hiemstra Maurice, Wickert Cristine, Prestes Osmar D.. Method validation for the analysis of 169 pesticides in soya grain, without clean up , by liquid chromatography–tandem mass spectrometry using positive and negative electrospray ionization[J]. Journal of Chromatography A, 2007, 1142: 123- 136.
Queiroz A A A, Ferraz H G, Abraham G A, et al. Development of new hydroactive dressings based on chitosan membranes:Characterization and in vivo behavior[J]. Journal of Biomedical Materials Research Part A,2003, 64A(1): 147-154.
Rezic I., Horvat A.J.M., Babic S., Kastelan-Macan M.. Determination of pesticides in honey by ultrasonic solvent extraction and thin-layer chromatography[J]. Ultrasonics Sonochemistry, 2005, 12: 477-481.
Richter B. E. , Ezzell J. L. , Felix D , Roberts K. A. , Later D. W.. An accelerated solvent extraction system for the rapid preparation of environmental organic compounds in soil[J]. American Laboratory , 1995, 27 (4) : 24-28.
Ridgway Kathy, Lalljie Sam P.D., Smith Roger M.. Sample preparationtechniques for the determination of trace residues and contaminants in foods[J]. Journal of Chromatography A, 2007, 1153: 36-53.
Rissato Sandra R., Galhianea Mario S., Knollb Fatima R.N., Apon Bernhard M.. Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with electron-capture and mass spectrometry detection[J]. Journal of Chromatography A, 2004, 1048: 153-159.
Sanusi Astrid, Guillet Valérie, Montury Michel. Advanced method using microwaves and solid-phase microextraction coupled with gas chromatography-mass spectrometry for the determination of pyrethroid residues in strawberries[J]. Journal of Chromatography A, 2004, 1046: 35-46.
Smalling Kelly L., Kuivila Kathryn M.. Multi-residue method for the analysis of 85 current-use and legacy pesticides in bed and suspended sediments [J].Journal of Chromatography A, 2008, 1210: 8-18.
Petr Suchan, PulkrabováJana, Haj?lováJ ana, Kocourek Vladimir. Pressurized liquid extraction in determination of polychlorinated biphenyls and organochlorine pesticides in fish samples[J]. Analytica Chimica Acta, 2004, 520: 193-200.
Valera Enrique, Ramón-Azcón Javier, Barranco Alejandro, Alfaro Bego?a, Francisco Sánchez-Baeza, Marco M.-P., Rodríguezángel. Determination of atrazine residues in red wine samples. A conductimetric solution[J]. Food Chemistry, 2010, 122: 888-894.
Van De Steene Jet C., Mortier Kjell A., Lambert Willy E.. Tackling matrix effects during development of a liquid Chromatographic-electrospray ionisation tandem mass spectrometric analysis of nine basic pharmaceuticals in aqueous environmental samples[J]. Journal of Chromatography A, 2006, 1123: 71-81.
Van De Steene Jet C. , Lambert Willy E.. Comparison of Matrix Effects in HPLC-MS/MS and UPLC-MS/MS Analysis of Nine Basic
Pharmaceuticals in Surface Waters[J]. Am Soc Mass Spectrom , 2008, 19: 713-718.
Wang Jian Hua, Xu Qiang, Jiao Kui. Supercritical fluid extraction and off-line clean-up for the analysis of organochlorine pesticide residues in garlic[J].Journal of Chromatography A, 1998, 818: 138-143.
Wang Yuanfeng , Du Ran. Simultaneous extraction of trace organophosphorous pesticides from plasma sample by automated solid phase extraction and determination by gas chromatography coupled with pulsed flame photometric detector[J]. Forensic Science International , 2010, 198: 70-73.
Watanabe H, Tanaka H. A nonionic surfactant as a new solvent for liquid- liquid extraction of Zinc ( II) with 1-(2-pyridylazo)-2-naphthol [J ]. Talanta, 1978, 25 (4): 585-589.
Wenclawiak B., Otterbach A.. Carbon-based quantitation of pyrethrins by supercritical-fluid chromatography[J ]. Biochem. Biophys. Methods , 2000, 43: 197-207.
Xie Shunping, Paaua Man Chin, Li Cheuk Fai, Xiao Dan, Choia Martin M.F.. Separation and preconcentration of persistent organic pollutants by cloud point extraction[J]. Journal of Chromatography A, 2010, 1217 : 2306- 2317.
Xu Dun-ming,Yang Fang, Lu Sheng-yu, Jin-Chang. Determination of indoxacarb residue in foodstuffs of plant and animal origin by GC-ECD and LC-MS/MS[J]. Agricultural Sciences in China, 2008, 7(10): 1228- 1234.
Yang Ruiqiang, Wang Yawei, Li An, Zhang Qinghua, Jing Chuanyong, Wang Thanh, Wang Pu, Li Yingming, Jiang Guibin. Organochlorine pesticides and PCBs in fish from lakes of the Tibetan Plateau and the implications[J]. Environmental Pollution , 2010, 158: 2310-2316.
You Jing, Wang Dongli, Lydy Michael J.. Determination of pyrethroid insecticides in sediment by gas chromatography-Ion trap tandem mass spectrometry[J].Talanta, 2010, 81: 136-141.
Zhang Hong ,Chen Zilei ,Yang Guosheng ,Wang Wenzheng ,Li Xiuqing , Li Ruiju ,Wu Yuanjuan. Microwave pretreatment and gas chromatography- mass spectrometry determination of herbicide residues in onion[J].Food Chemistry, 2008, 108: 322–328.
Zhao Limian, Lee Hian Kee. Application of static liquid-phase microextraction to the analysis of organochlorine pesticides in water[J]. Journal of Chromatography A, 2001, 919: 381-388.
Zhou Jihai, Chen Jiandong, Cheng Yanhong, Li Daming, Hu Feng, Li Huixin. Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction[J].Talanta, 2009, 79: 189-193.