QuEChERS在药用植物的农药多残留分析中的应用研究
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摘要
农药为保证农作物的丰产做出了巨大贡献,而农药的大量使用甚至是不合理使用势必造成农药残留现象。农作物中的农药残留对人畜健康和环境都造成很大的影响,而且,农药残留也逐渐成为阻碍我国农产品出口的重要原因。因此。开发建立农药多残留检测技术对人类健康和进出口贸易发展都有重要意义。
药用植物在其生长过程中,也要施用多种杀虫剂、杀菌剂,而目前我国药用植物的农药残留检测标准很少,残留限量要求很少,亟待开发检测技术。由于药物植物成分的特殊性使前处理过程更加复杂,QuEChERS自从2003年出现以来日益受到重视,该方法采用乙腈做为提取剂,PSA做为杂质吸附剂,应用于含水量较大的水果蔬菜等样品中,但随着方法的改进,已经广泛应用于各种基质的前处理中。本课题重点研究改进型分散固相萃取法应用于药用植物农药多残留前处理,使用液相色谱质谱联用检测,取得了很好的效果,主要研究结果如下:
1.在原有QuEChERS基础上,对提取净化条件进行逐项优化,最后确定采用1%乙酸的乙腈做为提取溶剂,无水硫酸镁做除水剂,均质提取,对于枸杞、山楂采用PSA、C18来做除杂剂,对于枳实还需加入少量GCB和甲苯去除色素,经过处理后的样品澄清并基本无色,适用于后续色质联用分析。与应用较为广泛的SPE(固相萃取)相比,QuEChERS在处理时间、前处理步骤、溶剂及填料使用量上都显示出明显的优越性,用时短,使用较少的仪器,对实验室要求很低,前处理成本也大大降低,
2.对LC-MS也进行了条件优化,使之适用于氨基甲酸酯类、苯酰脲类农药的检测,先直接进样优化质谱条件得到每种农药的定性定量离子,再优化HPLC条件。定性时,如果检出的色谱峰的保留时间与标准样品相一致,并且在扣除背景后的样品质谱图中,所选择的离子均出现,而且所选择的离子丰度比与标准样品的离子丰度比达到80%以上,则可判断样品中存在这种农药。采用外标-校准曲线法定量测定。为减少基质对定量测定的影响,需用空白样液来配制所使用的一系列基质标准工作溶液,用基质标准工作溶液分别进样绘制标准曲线。用绘制的校准曲线对样品进行定量。
3.通过加标回收试验证实,改进后的方法具有很高的回收率和较小的相对标准偏差,可以做为药用植物中常用农药的多残留检测。
The use of pesticides provides unquestionable benefits in increasing agricultural production, however, the problem of pesticide residues has potential risk to consumers and pesticide residues become one of the obstructions china’s productions to export.
Chinese herbal medicine used some pesticides and fungicide during its growth and in china today there is few test technique about Chinese herbal medicine, so take some research on the technique of pesticide residues test will have significance on the improving of exportation. As the special composition of herbal medicine, it will be more complex for the pretreatment. QuEChERS was more and more popular science 2003, which uses acetonitrile as extract solvent, PSA as sorbent, it was used in fruits and vegetables, but with more modified methods were developed, it was used in more and more matrixes. In this study, I mainly discussed how to modify the method so that it can be used in the multi-residue test of Chinese herbal medicine. This study used LC-MS/MS, and the results can fulfill the daily test. Consequences are as follows:
1. Based on the original QuEChERS,optimized the extract and purification steps one by one, in the end ,I choose 1% acetic acid in acetonitrile as extract solvent, anhydrous magnesium sulfate to remove water in matrix, homogeneity extraction, for wolfberry, PSA、C18 was used as sorbent, however, citrus uranium ,GCB and toluene must be used to remove pigment. The extract was brilliantly clear after the pretreatment. Compared with SPE, QuEChERS cost little time and less glass ware, requirement of the laboratory is very low, greatly reduced the cost of pretreatment, so it can be widely used in many laboratories.
2. Optimized the LC-MS/MS conditions, make it fit for the carbamate pesticides and benzoyl urea insecticides. Firstly, optimize the MS conditions, then the HPLC conditions. This method used ion for qualitative and standard curve for quantitfication, For accurate quantitative, I made a standard curve according to the blank matrix.
3. Confirmed by standard recovery, the modified QuEChERS method has good recoveries and smaller standard deviation, can be used on the determination of multi-pesticides residue in Chinese herbal medicine
药用植物在其生长过程中,也要施用多种杀虫剂、杀菌剂,而目前我国药用植物的农药残留检测标准很少,残留限量要求很少,亟待开发检测技术。由于药物植物成分的特殊性使前处理过程更加复杂,QuEChERS自从2003年出现以来日益受到重视,该方法采用乙腈做为提取剂,PSA做为杂质吸附剂,应用于含水量较大的水果蔬菜等样品中,但随着方法的改进,已经广泛应用于各种基质的前处理中。本课题重点研究改进型分散固相萃取法应用于药用植物农药多残留前处理,使用液相色谱质谱联用检测,取得了很好的效果,主要研究结果如下:
1.在原有QuEChERS基础上,对提取净化条件进行逐项优化,最后确定采用1%乙酸的乙腈做为提取溶剂,无水硫酸镁做除水剂,均质提取,对于枸杞、山楂采用PSA、C18来做除杂剂,对于枳实还需加入少量GCB和甲苯去除色素,经过处理后的样品澄清并基本无色,适用于后续色质联用分析。与应用较为广泛的SPE(固相萃取)相比,QuEChERS在处理时间、前处理步骤、溶剂及填料使用量上都显示出明显的优越性,用时短,使用较少的仪器,对实验室要求很低,前处理成本也大大降低,
2.对LC-MS也进行了条件优化,使之适用于氨基甲酸酯类、苯酰脲类农药的检测,先直接进样优化质谱条件得到每种农药的定性定量离子,再优化HPLC条件。定性时,如果检出的色谱峰的保留时间与标准样品相一致,并且在扣除背景后的样品质谱图中,所选择的离子均出现,而且所选择的离子丰度比与标准样品的离子丰度比达到80%以上,则可判断样品中存在这种农药。采用外标-校准曲线法定量测定。为减少基质对定量测定的影响,需用空白样液来配制所使用的一系列基质标准工作溶液,用基质标准工作溶液分别进样绘制标准曲线。用绘制的校准曲线对样品进行定量。
3.通过加标回收试验证实,改进后的方法具有很高的回收率和较小的相对标准偏差,可以做为药用植物中常用农药的多残留检测。
The use of pesticides provides unquestionable benefits in increasing agricultural production, however, the problem of pesticide residues has potential risk to consumers and pesticide residues become one of the obstructions china’s productions to export.
Chinese herbal medicine used some pesticides and fungicide during its growth and in china today there is few test technique about Chinese herbal medicine, so take some research on the technique of pesticide residues test will have significance on the improving of exportation. As the special composition of herbal medicine, it will be more complex for the pretreatment. QuEChERS was more and more popular science 2003, which uses acetonitrile as extract solvent, PSA as sorbent, it was used in fruits and vegetables, but with more modified methods were developed, it was used in more and more matrixes. In this study, I mainly discussed how to modify the method so that it can be used in the multi-residue test of Chinese herbal medicine. This study used LC-MS/MS, and the results can fulfill the daily test. Consequences are as follows:
1. Based on the original QuEChERS,optimized the extract and purification steps one by one, in the end ,I choose 1% acetic acid in acetonitrile as extract solvent, anhydrous magnesium sulfate to remove water in matrix, homogeneity extraction, for wolfberry, PSA、C18 was used as sorbent, however, citrus uranium ,GCB and toluene must be used to remove pigment. The extract was brilliantly clear after the pretreatment. Compared with SPE, QuEChERS cost little time and less glass ware, requirement of the laboratory is very low, greatly reduced the cost of pretreatment, so it can be widely used in many laboratories.
2. Optimized the LC-MS/MS conditions, make it fit for the carbamate pesticides and benzoyl urea insecticides. Firstly, optimize the MS conditions, then the HPLC conditions. This method used ion for qualitative and standard curve for quantitfication, For accurate quantitative, I made a standard curve according to the blank matrix.
3. Confirmed by standard recovery, the modified QuEChERS method has good recoveries and smaller standard deviation, can be used on the determination of multi-pesticides residue in Chinese herbal medicine
引文
1.安捷伦科技有限公司.液相/电喷雾飞行时间质谱和液相/电喷雾离子阱质谱测定水果和蔬菜中的杀真菌剂.环境化学,2005,24(4):486～490.
2.陈小华,汪群杰.固相萃取技术与应用.北京:科学出版社,1～4,156～160.
3.陈燕清,谢石宇,颜流水,魏洽.液相色谱/质谱法测定生鲜牛奶中的两种氨基甲酯农药残留.江西科学,2006,24(3): 242～244,248.
4.陈建荣,田文玉.固相萃取-气相色谱法测定饲料中13种有机氯农药残留量.饲料工业,2009,30(17):45～46.
5.丁岚,谢孟峡,刘媛,单吉浩,杨清峰,刘素英.高效液相色谱法测定鸡蛋中呋喃唑酮的残留量.分析化学.2004,32(2):139～142.
6.董顺玲,胡家炽,何志强.中药材中氨基甲酸酯类农药残留量的反高校液相色谱.药物分析杂志,2002,22 (3):l78～182.
7.傅水玉,陈晓生,王明,王成.气相色谱法测定茶叶中有机氯农药残留的前处理方法研究.杭州师范学院学报(自然科学版),2006,5(2):118～122.
8.冯秀琼,汤庆勇.中草药中14种有机磷农药残留量同时测定—微波辅助提取法.农药学报,2001,3:47～52.
9.国家药典委员会.中华人民共和国药典.北京:化学工业出版社,2000,附录60.
10.国家食品药品监督管理局.《中药材生产质量管理规范认证管理办法》.北京:2003.
11.宫兆晶.基质固相分散-气相色谱法测定油菜籽中有机磷农药残留检测技术研究.北京:中国农业科学院,2006.
12.高文惠,艾连峰.高效液相色谱-串联质谱法测定进出口食品中十三吗啉残留.食品科学,2009,30(22): 331～334.
13.何笑荣,邹定,冯金红,吴学军,胡欣,孙春华.固相萃取/GC /MS测定金银花中有机磷农药残留量.中国药学杂志,2007,42(24):1901～1904.
14.胡西洲,程运斌,胡定金. QuEChERS法测定蔬菜中有机磷类农药多残留分析.中国测试技术,2006,32(3):132～133.
15.胡西洲,程运斌,胡定金.农药多残留分析中的QuEChERS方法介绍.现代农药,2006,5(4):24～29.
16.黄惠玲,张薇君,丁慧瑛.气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留.分析测试通报,2006,25(4):81～82.
17.黄百芬,张文娟,沈向红.高效液相色谱法同时测定酱油或饮料中的8种防腐剂和3种甜味剂.中国卫生检验杂志,2005,15(10): 1208～1210.
18.何强,孔祥虹,赵洁,李建华,乐爱山.SPE—HPLC法同时测定浓缩苹果汁中四螨嗪等4种农药的残量.分析试验室,2008,27(7):54～57.
19.贺利民,刘祥国,曹振灵.气相色谱分析农药残留的基质效应及其解决方法.色谱,2008,26(1):98～104.
20.金雁,姜莉,林颖,赵颖.高效液相色谱法测定畜禽肉中四环素族抗生素的残留量.沈阳师范大学学报(自然科学版),2006,24(2):218～220.
21.贾丽莉.固相萃取气相色谱法测定水中痕量有机磷农药.黑龙江水利科技,2009(5):50～51.
22.李竺,陈玲,郜洪文,董丽娴,赵建夫.固相萃取-高效液相色谱法测定环境水样中的三嗪类化合物色谱, 2006, 24(3): 267～270.
23.李晶,董丰收,刘新刚,姚建仁,郑永权.我国中药材中农药残留现状及其对策.农药研究与应用,2008,12(1):12～15.
24.李小平,蒋经伟,范建中,金米聪,姚浔平.固相萃取HPLC法测定豆芽中4-氯苯氧乙酸钠.中国卫生检验杂志,2006,16(3): 267～269.
25.李莉,江树人,潘灿平,等.分散固相萃取-气相色谱-质谱方法快速净化测定枸杞中12种农药残留.农药学学报,2006,8 (4) :371～374.
26.刘咏梅,王志华,储晓刚.凝胶渗透色谱技术在农药残留分析中的应用.分析测试学报,2005,24(2):123～127.
27.李文秀,徐可欣,汪嚥,等.蔬菜农药残留检测的红外光谱法研究.光谱学与光谱分析,2004,24(10):1202～1204.
28.李欢欣,赵春杰,沈艳霞.超临界流体萃取法净化黄芪中有机氯农药的研究.中国药学杂志, 2005,40(17):1335～1339.
29.刘文长陶文靖程丽娅余兴田旻黄勤等.超声提取-固相萃取小柱净化-气相色谱法测定土壤中14种有机氯农药.岩矿测试.2009,28(6):541～544.
30.马涛.农药残留检测中现代前处理技术的应用.山西农业科学,2007,35(2):80～82.
31.沈昊宇,应丽艳,曹云峰,潘刚,周鹿.固相萃取-气相色谱/质谱法同时测定化妆品中的邻苯
二甲酸酯和对羟基苯甲酸.色谱,2007,25(2):272～275.
32.沈红,钱大玮,段金廒.SPE-HPLC-ELSD法测定黄芪中黄芪甲苷的含量.现代中药研究与实践,2006,20(1):45～49.
33.沈菁,程运斌,刘军等.分散固相萃取-高效液相色谱-质谱联用法测定大米中的呋喃丹残留.现代科学仪器,2008,2:66～68.
34.谭力,鞠熀先,黎介寿,周敏,李小双,柳晓泉.血清总磷脂脂肪酸组分的固相萃取-气相色谱法分析.分析科学学报.2006,22(2):125～128.
35.万益群,毛雪金,鄢爱平.微波辅助提取_气相色谱法同时测定中草药中有机磷和氨基甲酸酯农药残留.分析科学学报.2009,25(5):537～542.
36.王大宁,董益阳,邹明强.农药残留检测与监控技术.北京:化学工业出版社,2006,1～10.
37.王素利,潘灿平,李莉,江树人,钱传范,刘丰茂.水果蔬菜中多种杀菌剂的基质固相分散液
38.相色谱测定方法研究.分析测试学报,2007,26(6):808～812.
39.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,农业质量标,2007 (1):28～31.
40.王艳萍,汪心想,任保增.超临界流体萃取技术的应用.河南化工,2009,26(12):25～27.
41.王亚飞.农药残留速测技术研究进展.世界农药,2009,31(1):42～45.
42.徐维海,张干,邹世春,李向东,刘玉春.固相萃取-液相色谱/串联质谱法分析水体中痕量抗生素.环境化学,2006,25(2): 232～233.
43.薛健,杨世林,陈建民,张丽萍,马小军.我国中药材农药残留污染现状与对策.2001,26(9):637～641.
44.向增旭,赵维佳2,郭巧生金银花中18种有机磷农药残留量分析方法的研究中国中药杂志.2006,31(16):131～134.
45.熊飞,陈玲,马娜.水中几种有机污染物的SPE-HPLC联用测定技术环境科学与技术.2002,25(5):17～21.
46.薛凤丽,李岩,杨瑞强,胡长荣,张福全,丁文军,徐裕良.SPME-HPLC法测定水中的酚类化合物.中国给水排水,2006,22(16): 81～83.
47.向平,沈敏,卓先义.液相色谱一质谱分析中的基质效应.分析测试学报, 2009,28(6):753～756.
48.岳霞丽,张新萍,董元彦.固相萃取-高效液相色谱法测定藻液中甲磺隆的残留量.化学与生物工程,2006,23(3):54～55.
49.姚海波,韩国君,刘国霞,谢彦.SPE-HPLC方法分析灭草喹在大米中的残留.安徽农业科学,2009,37(20):9326～9327,9329.
50.中华人民共和国商务部.WM/T2-2004.药用植物及制剂进出口绿色行业标准.北京:中国标准出版社,2005.
51.中华人民共和国国家质量监督检验检疫总局.GB/T 23200-2008.桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法.北京:中国标准出版社,2009.
52.赵华,胡秀卿,吴珉,彭金波.基质固相分散-加速溶剂萃取-气相色谱法测定土壤中六六六
53.和滴滴涕农药残留.浙江农业科学,2008(3):339～341.
54.郑锋,庞国芳,李岩,王明林,范春林.凝胶渗透色谱净化气相色谱-质谱法检测河豚鱼、鳗鱼和对虾中191种农药残留.色谱,2009,27(5):700～710.
55.周向阳,林纯忠,胡祥娜,金同铭,王瑞,林润昌.近红外光谱法(NIR)快速诊断蔬菜中有机磷农药残留.食品科学,2004,25,(5): 151～155.
56.周艳明,付婷,胡睿,田宏哲.气相色谱法对水果样品中三碘苯甲酸残留的测定.分析测试学报,2009,28(11):1283～1286.
57.张荷丽,张卢军,马婧玮,潘灿平.QuEChERS/GC-MS检测土壤中POPs的含量.分析测试学报,2006,:151～152.
58.赵鹏飞,李柏林.SPE-HPLC法分析大鼠血浆中灭多威.中国法医学杂志,2009,24(6):386～3 88.
59.中华人民共和国农业部.NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留检测方法.北京:中国标准出版社:2008.
60.中华人民共和国农业部.NY/T 1380-2007蔬菜、水果中51种农药多残留的测定气相色谱质谱法.北京:中国标准出版社:2007.
61. Anastassiades M,Lehotay S J,Stajnbaher.Fast and easy multiresidue method employing
62. acetonitrile extraction/partitioning an“dispensive solid-Phase extraction”for the determination of pesticide residues in produce.J.AOAC Int.
63. András Székács, Hong T.M. Le, Ferenc Szurdoki, Bruce D.Hammock.Optimization and validation of an enzyme immunoassay for the insect growth regulator fenoxycarb.Analytica Chimica Acta, 2003(487):15～29.
64. Ana Isabel García-Valcárcel, JoséLuis Tadeo. A combination of ultrasonic assisted extraction with LC–MS/MS for the determination of organophosphorus pesticides in sludge.Analytica Chimica Acta, 2009, 641:117～123.
65. Anneli Kruve, Allan K¨unnapas, Koit Herodes, Ivo Leito.Matrix effects in pesticide multi-residue analysis by liquid chromatography–mass spectrometry.Journal of Chromatography A, 2008,1187 :58～66.
66. C. D′?ez, W.A. Traag, P. Zommer, P. Marinero, J. Atienza.Comparison of an acetonitrile extraction/partitioning and“dispersive solid-phase extraction”method with classical multi-residue methods for the extraction of herbicide residues in barley samples. Journal of Chromatography A, 2006,(1131):11～23.
67. Carmen Ferrer, M.Jose G′omez,Juan F.Garc′?a-Reyes,Imma Ferrer, E.Michael Thurman,Amadeo R. Fern′andez-Alba. Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry.Journal of Chromatography A, 2005,1069:183～194.
68. EN 15662 version 2007-10-24, Food of Plant origin-determination of pesticides residues using GC-MS and /or LC-MS/MS following Acetonitrile Extraction/Partitioning and Clean-up by Disperse SPE (QuEChERS method).
69. E. Peter Maziarz, Michael Liu, Edmond T.Quinn,Yu-Chin Lai,Daniel M. Ammon, Jr.,George L. Grobe. Detailed Analysis of Bis(4-hydroxybutyl) Poly(dimethylsiloxane) Using GPC-MALDI TOF Mass Spectrometry.Mass Spectrom, 2002, 13:170～176.
70. F. Gores,P. Montag,C.Schall,J. Vienken,S.K.Bowry.Verificat specifications of haemodialysis membranes by NMR and GPC-FTIR-coupled spectroscopy .Biomaterials.2002,(23):3131～3140.
71. Gunter G.C, Kuhnle a,Caterina Dell’Aquila ,Sue M,Aspinall,Shirley A, Runswick ,Annemiek M.C.P. Joosen, Angela. Mulligan, Sheila. Bingham .Phytoestrogen content of fruits and vegetables commonly consumed in the UK based on LC–MS and 13C-labelled standards.Food Chemistry, 2009,116:542～554.
72. Guo-Fang Pang ,Yan-Zhong Cao, Jin-Jie Zhang, Chun-Lin Fan, Yong-Ming Liu, Xue-Min Li,et al.Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry .Journal of Chromatography A, 2006, 1125:1～30.
73. Gaurav, Varinder Kaur, Ashwini Kumar, Ashok Kumar Malik, P.K.Rai. SPME-HPLC: A new approach to the analysis of explosives. Journal of Hazardous Materials. 2007, 147 691–697.
74. Hao-Yu Shen, Hai-Liang Jiang .Screening, determination and confirmation of chloramphenicol in seafood, meat and honey using ELISA, HPLC–UVD, GC–ECD, GC–MS–EI–SIM and GCMS–NCI–SIM methods. Analytica Chimica Acta, 2005,535:33～41.
75. Jeong-Min Lee, Jin-Won Park, Gi-Chul Jang, Keon-Joong Hwang .Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry.Journal of Chromatography A,2008 (1187):25～33.
76. Jasna Dmitrovic, Siu C. Chan, Sylvia H.Y. Chan. Analysis of pesticides and PCB congeners in serum by GC/MS with SPE sample cleanup.Toxicology Letters 2002(134):253～258.
77. Jeong-Min Lee, Jin-Won Park, Gi-Chul Jang, Keon-Joong Hwang.Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry. Journal of Chromatography A, 2008(1187): 25～33.
78. Koichi Inoue, Shiho Murayama, Kazue Takeba,Yoshihiro Yoshimura, Hiroyuki Nakazawa.Contamination of xenoestrogens bisphenol A and F in honey:safety assessment and analytical method of these compounds in honey.Journal of Food Composition and Analysis, 2003(16):497～506.
79. Liyan Liao,Ji Yang,Yalin Wang, Tonghua Sun,Jinping Jia.Study on a novel circulating cooling solid-phase microextraction method. Journal of Chromatography A,2006,1135:1～5.
80. Li-Fei Wang, Joo-Yeon Lee , Jin-Oh Chung, Joo-Hyun Baik,Sung So, Seung-Kook Park.Discrimination of teas with different degrees of fermentation by SPME–GC analysis of the characteristic volatile flavour compounds.Food Chemistry,2008,(109):196～206.
81. Liu Junting, Cheng Peng1, O. Suzuki .Solid-phase microextraction (SPME) of drugs and poisons from biological samples.Forensic Science International, 1998,97:93～100.
82. Lehotay S J, Kok A, Hiemstra M, et al. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectro-metric detection. J of AOAC Int, 2005, 88(2): 595～614.
83. Min Liu, Yuki Hashi, Yuanyuan Song, Jin-Ming Lin.Simultaneousdetermination of carbamate and organophosphorus pesticides in fruits and vegetables by liquid chromatography–mass spectrometry.Journal of Chromatography A, 2005(1097):183～187.Ion of the chemical composition and
84. Marina Radi?ic′, Svetlana Grujic′, Tatjana Vasiljevic′, Mila Lau?evic .Determination of selected pesticides in fruit juices by matrix solid-phase dispersion and liquid chromatography–tandem mass spectrometry.Food Chemistry2009, 113:712～719.
85. M M Aguilera-Luiz, Jose Luis Martínez Vidal, Roberto Romero-González. Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography–tandem mass spectrometry.Journal of Chromatography A, 2008, 1205:10～16.
86. P.C. Abhilash, Vandana Singh, Nandita Singh.Simplified determination of combined residues of lindane and other HCH isomers in vegetables, fruits, wheat, pulses and medicinal plants by matrix solid-phase dispersion (MSPD) followed by GC–ECD.Food Chemistry, 2009, (113):267～271.
87. Paula Payá,Michelangelo Anastassiades,Dorothea Mack,et al. Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem, 2007, 389:1697～1714.
88. QuEChERS:A mini-multiresidue method for the analysis of pesticides residue in low-fat products.retrieved from www. QuEChERS.com, 2009.
89. Ronald E.Majors. QuEChERS-A New Technique for Multiresidue Analysis of Pesticides in Foods and Agricultural Samples.LC-GC Asia Pacific,2008,11(1):22～31.
90. Robert Loos,Giovanni Locoro, Serafino Contini .Occurrence of polar organic contaminants in the dissolved water phase of the Danube River and its major tributaries using SPE-LC-MS2 analysis .Water Research, 2010, 44(7):2325～2335.
91. Raquel Andrade,Felix G.R. Reyes, Susanne Rath.A method for the determination of volatile N-nitrosamines in food by HS-SPME-GC-TEA.Food Chemistry, 2005,(91):173～179.
92. Steven A.Barker.Applications of matrix solid-phase dispersion in food analysis. Journal of Chromatography A,2000,880:63～68.
93. Schenck, F J, Brown A N, Podhorniak L V, Parker A, Reliford M, Wong J W. A rapid multiresidue method for determination of pesticides in fruits and vegetables by using Acetonitrile Extraction/Partitioning and solid phage extraction column Clean-up. J.AOAC Int,2008,91 (2):422～438.
94. Szilard Szilagyi,Beatriz de la Calle.Development and validation of an analytical method for the determination of semicarbazide in fresh egg and in egg powder based on the use of liquid chromatography tandem mass spectrometry.Analytica Chimica Acta, 2006,572:113～120.
95. The novel radical scavenger IAC is effective in preventing and protecting against post-ischemic brain damage in Mongolian gerbils Donatella Canistro, Alessandra A. Affatato, Antonio Soleti, Vincenzo Mollace, Carolina Muscoli, Francesca Sculco, et al. Journal of the Neurological Sciences 2010(290):90～95.
96. Thanh Dong Nguyen, Ji Eun Yu, Dae Myung Lee, Gae-Ho Lee. A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry.Food Chemistry, 2008, (110):207～213.
97. Thierry Dagnac, Maria Garcia-Chao, Paula Pulleiro, Carmen Garc solid-phase extraction followed by liquid chromatography–tandemmass spectrometry for the multi-residue analysis of pesticides in raw bovine milk.Journal of Chromatography A, 2009,1216:3702～3709.
98. Tomas Cajka, Jana Hajslova, Ondrej Lacina. Rapid analysis of multiple pesticide residues in fruit-based baby food using programmed temperature vaporizer injection–low-pressure gas chromatography–high-resolution time-of-flight mass spectrometry. Journal of Chromatography A, 2008, 1186: 281～294.
99. Vimal K, Balakrishnan, Ken A. Terry John Toito.Determination of sulfonamide antibiotics in wastewater: A comparison of solid phase microextraction and solid phase extraction methods.Journal of Chromatography A, 2006, 1131, 1～10.
100. XU Dun-ming,YANG Fang,LU Sheng-yu, LAN Jin-chang,YU Kong-jie,CAI Chun-ping,et al.Determination of Indoxacarb Residue in Foodstuffs of Plant and Animal Origin by GC-ECD and LC-MS/MS.Agricultural Sciences in China,2008, 7(10):1228～1234.
101. yagiie C ,bayarri S,lazaro R,conchello P,Arino,Herrera A. J.AOAC Int.2001,84:1561.
102. Zsuzsanna Kuklenyik, Xavier A. Bryant, Larry L, Needham, Antonia M. Calafat.SPE/SPME–GC/MS approach for measuring musk compounds in serum and breast milk.Journal of Chromatography B, 2007,858:177～183.
103. ZENG Dong-ping, LIN Cui-ping, ZENG Zhen-ling, HUANG Xian-hui and HE Li-min.Multi-Residue Determination of Eight Anabolic Steroids by GC-MS in Muscle Tissues from Pigs. Agricultural Sciences in China, 2010, 9(2): 306-312.ia-Jares, Maria Llompart Dispersive.
2.陈小华,汪群杰.固相萃取技术与应用.北京:科学出版社,1～4,156～160.
3.陈燕清,谢石宇,颜流水,魏洽.液相色谱/质谱法测定生鲜牛奶中的两种氨基甲酯农药残留.江西科学,2006,24(3): 242～244,248.
4.陈建荣,田文玉.固相萃取-气相色谱法测定饲料中13种有机氯农药残留量.饲料工业,2009,30(17):45～46.
5.丁岚,谢孟峡,刘媛,单吉浩,杨清峰,刘素英.高效液相色谱法测定鸡蛋中呋喃唑酮的残留量.分析化学.2004,32(2):139～142.
6.董顺玲,胡家炽,何志强.中药材中氨基甲酸酯类农药残留量的反高校液相色谱.药物分析杂志,2002,22 (3):l78～182.
7.傅水玉,陈晓生,王明,王成.气相色谱法测定茶叶中有机氯农药残留的前处理方法研究.杭州师范学院学报(自然科学版),2006,5(2):118～122.
8.冯秀琼,汤庆勇.中草药中14种有机磷农药残留量同时测定—微波辅助提取法.农药学报,2001,3:47～52.
9.国家药典委员会.中华人民共和国药典.北京:化学工业出版社,2000,附录60.
10.国家食品药品监督管理局.《中药材生产质量管理规范认证管理办法》.北京:2003.
11.宫兆晶.基质固相分散-气相色谱法测定油菜籽中有机磷农药残留检测技术研究.北京:中国农业科学院,2006.
12.高文惠,艾连峰.高效液相色谱-串联质谱法测定进出口食品中十三吗啉残留.食品科学,2009,30(22): 331～334.
13.何笑荣,邹定,冯金红,吴学军,胡欣,孙春华.固相萃取/GC /MS测定金银花中有机磷农药残留量.中国药学杂志,2007,42(24):1901～1904.
14.胡西洲,程运斌,胡定金. QuEChERS法测定蔬菜中有机磷类农药多残留分析.中国测试技术,2006,32(3):132～133.
15.胡西洲,程运斌,胡定金.农药多残留分析中的QuEChERS方法介绍.现代农药,2006,5(4):24～29.
16.黄惠玲,张薇君,丁慧瑛.气相色谱-质谱大体积进样法测定蔬菜、水果中17种农药残留.分析测试通报,2006,25(4):81～82.
17.黄百芬,张文娟,沈向红.高效液相色谱法同时测定酱油或饮料中的8种防腐剂和3种甜味剂.中国卫生检验杂志,2005,15(10): 1208～1210.
18.何强,孔祥虹,赵洁,李建华,乐爱山.SPE—HPLC法同时测定浓缩苹果汁中四螨嗪等4种农药的残量.分析试验室,2008,27(7):54～57.
19.贺利民,刘祥国,曹振灵.气相色谱分析农药残留的基质效应及其解决方法.色谱,2008,26(1):98～104.
20.金雁,姜莉,林颖,赵颖.高效液相色谱法测定畜禽肉中四环素族抗生素的残留量.沈阳师范大学学报(自然科学版),2006,24(2):218～220.
21.贾丽莉.固相萃取气相色谱法测定水中痕量有机磷农药.黑龙江水利科技,2009(5):50～51.
22.李竺,陈玲,郜洪文,董丽娴,赵建夫.固相萃取-高效液相色谱法测定环境水样中的三嗪类化合物色谱, 2006, 24(3): 267～270.
23.李晶,董丰收,刘新刚,姚建仁,郑永权.我国中药材中农药残留现状及其对策.农药研究与应用,2008,12(1):12～15.
24.李小平,蒋经伟,范建中,金米聪,姚浔平.固相萃取HPLC法测定豆芽中4-氯苯氧乙酸钠.中国卫生检验杂志,2006,16(3): 267～269.
25.李莉,江树人,潘灿平,等.分散固相萃取-气相色谱-质谱方法快速净化测定枸杞中12种农药残留.农药学学报,2006,8 (4) :371～374.
26.刘咏梅,王志华,储晓刚.凝胶渗透色谱技术在农药残留分析中的应用.分析测试学报,2005,24(2):123～127.
27.李文秀,徐可欣,汪嚥,等.蔬菜农药残留检测的红外光谱法研究.光谱学与光谱分析,2004,24(10):1202～1204.
28.李欢欣,赵春杰,沈艳霞.超临界流体萃取法净化黄芪中有机氯农药的研究.中国药学杂志, 2005,40(17):1335～1339.
29.刘文长陶文靖程丽娅余兴田旻黄勤等.超声提取-固相萃取小柱净化-气相色谱法测定土壤中14种有机氯农药.岩矿测试.2009,28(6):541～544.
30.马涛.农药残留检测中现代前处理技术的应用.山西农业科学,2007,35(2):80～82.
31.沈昊宇,应丽艳,曹云峰,潘刚,周鹿.固相萃取-气相色谱/质谱法同时测定化妆品中的邻苯
二甲酸酯和对羟基苯甲酸.色谱,2007,25(2):272～275.
32.沈红,钱大玮,段金廒.SPE-HPLC-ELSD法测定黄芪中黄芪甲苷的含量.现代中药研究与实践,2006,20(1):45～49.
33.沈菁,程运斌,刘军等.分散固相萃取-高效液相色谱-质谱联用法测定大米中的呋喃丹残留.现代科学仪器,2008,2:66～68.
34.谭力,鞠熀先,黎介寿,周敏,李小双,柳晓泉.血清总磷脂脂肪酸组分的固相萃取-气相色谱法分析.分析科学学报.2006,22(2):125～128.
35.万益群,毛雪金,鄢爱平.微波辅助提取_气相色谱法同时测定中草药中有机磷和氨基甲酸酯农药残留.分析科学学报.2009,25(5):537～542.
36.王大宁,董益阳,邹明强.农药残留检测与监控技术.北京:化学工业出版社,2006,1～10.
37.王素利,潘灿平,李莉,江树人,钱传范,刘丰茂.水果蔬菜中多种杀菌剂的基质固相分散液
38.相色谱测定方法研究.分析测试学报,2007,26(6):808～812.
39.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,农业质量标,2007 (1):28～31.
40.王艳萍,汪心想,任保增.超临界流体萃取技术的应用.河南化工,2009,26(12):25～27.
41.王亚飞.农药残留速测技术研究进展.世界农药,2009,31(1):42～45.
42.徐维海,张干,邹世春,李向东,刘玉春.固相萃取-液相色谱/串联质谱法分析水体中痕量抗生素.环境化学,2006,25(2): 232～233.
43.薛健,杨世林,陈建民,张丽萍,马小军.我国中药材农药残留污染现状与对策.2001,26(9):637～641.
44.向增旭,赵维佳2,郭巧生金银花中18种有机磷农药残留量分析方法的研究中国中药杂志.2006,31(16):131～134.
45.熊飞,陈玲,马娜.水中几种有机污染物的SPE-HPLC联用测定技术环境科学与技术.2002,25(5):17～21.
46.薛凤丽,李岩,杨瑞强,胡长荣,张福全,丁文军,徐裕良.SPME-HPLC法测定水中的酚类化合物.中国给水排水,2006,22(16): 81～83.
47.向平,沈敏,卓先义.液相色谱一质谱分析中的基质效应.分析测试学报, 2009,28(6):753～756.
48.岳霞丽,张新萍,董元彦.固相萃取-高效液相色谱法测定藻液中甲磺隆的残留量.化学与生物工程,2006,23(3):54～55.
49.姚海波,韩国君,刘国霞,谢彦.SPE-HPLC方法分析灭草喹在大米中的残留.安徽农业科学,2009,37(20):9326～9327,9329.
50.中华人民共和国商务部.WM/T2-2004.药用植物及制剂进出口绿色行业标准.北京:中国标准出版社,2005.
51.中华人民共和国国家质量监督检验检疫总局.GB/T 23200-2008.桑枝、金银花、枸杞子和荷叶中488种农药及相关化学品残留量的测定气相色谱-质谱法.北京:中国标准出版社,2009.
52.赵华,胡秀卿,吴珉,彭金波.基质固相分散-加速溶剂萃取-气相色谱法测定土壤中六六六
53.和滴滴涕农药残留.浙江农业科学,2008(3):339～341.
54.郑锋,庞国芳,李岩,王明林,范春林.凝胶渗透色谱净化气相色谱-质谱法检测河豚鱼、鳗鱼和对虾中191种农药残留.色谱,2009,27(5):700～710.
55.周向阳,林纯忠,胡祥娜,金同铭,王瑞,林润昌.近红外光谱法(NIR)快速诊断蔬菜中有机磷农药残留.食品科学,2004,25,(5): 151～155.
56.周艳明,付婷,胡睿,田宏哲.气相色谱法对水果样品中三碘苯甲酸残留的测定.分析测试学报,2009,28(11):1283～1286.
57.张荷丽,张卢军,马婧玮,潘灿平.QuEChERS/GC-MS检测土壤中POPs的含量.分析测试学报,2006,:151～152.
58.赵鹏飞,李柏林.SPE-HPLC法分析大鼠血浆中灭多威.中国法医学杂志,2009,24(6):386～3 88.
59.中华人民共和国农业部.NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留检测方法.北京:中国标准出版社:2008.
60.中华人民共和国农业部.NY/T 1380-2007蔬菜、水果中51种农药多残留的测定气相色谱质谱法.北京:中国标准出版社:2007.
61. Anastassiades M,Lehotay S J,Stajnbaher.Fast and easy multiresidue method employing
62. acetonitrile extraction/partitioning an“dispensive solid-Phase extraction”for the determination of pesticide residues in produce.J.AOAC Int.
63. András Székács, Hong T.M. Le, Ferenc Szurdoki, Bruce D.Hammock.Optimization and validation of an enzyme immunoassay for the insect growth regulator fenoxycarb.Analytica Chimica Acta, 2003(487):15～29.
64. Ana Isabel García-Valcárcel, JoséLuis Tadeo. A combination of ultrasonic assisted extraction with LC–MS/MS for the determination of organophosphorus pesticides in sludge.Analytica Chimica Acta, 2009, 641:117～123.
65. Anneli Kruve, Allan K¨unnapas, Koit Herodes, Ivo Leito.Matrix effects in pesticide multi-residue analysis by liquid chromatography–mass spectrometry.Journal of Chromatography A, 2008,1187 :58～66.
66. C. D′?ez, W.A. Traag, P. Zommer, P. Marinero, J. Atienza.Comparison of an acetonitrile extraction/partitioning and“dispersive solid-phase extraction”method with classical multi-residue methods for the extraction of herbicide residues in barley samples. Journal of Chromatography A, 2006,(1131):11～23.
67. Carmen Ferrer, M.Jose G′omez,Juan F.Garc′?a-Reyes,Imma Ferrer, E.Michael Thurman,Amadeo R. Fern′andez-Alba. Determination of pesticide residues in olives and olive oil by matrix solid-phase dispersion followed by gas chromatography/mass spectrometry and liquid chromatography/tandem mass spectrometry.Journal of Chromatography A, 2005,1069:183～194.
68. EN 15662 version 2007-10-24, Food of Plant origin-determination of pesticides residues using GC-MS and /or LC-MS/MS following Acetonitrile Extraction/Partitioning and Clean-up by Disperse SPE (QuEChERS method).
69. E. Peter Maziarz, Michael Liu, Edmond T.Quinn,Yu-Chin Lai,Daniel M. Ammon, Jr.,George L. Grobe. Detailed Analysis of Bis(4-hydroxybutyl) Poly(dimethylsiloxane) Using GPC-MALDI TOF Mass Spectrometry.Mass Spectrom, 2002, 13:170～176.
70. F. Gores,P. Montag,C.Schall,J. Vienken,S.K.Bowry.Verificat specifications of haemodialysis membranes by NMR and GPC-FTIR-coupled spectroscopy .Biomaterials.2002,(23):3131～3140.
71. Gunter G.C, Kuhnle a,Caterina Dell’Aquila ,Sue M,Aspinall,Shirley A, Runswick ,Annemiek M.C.P. Joosen, Angela. Mulligan, Sheila. Bingham .Phytoestrogen content of fruits and vegetables commonly consumed in the UK based on LC–MS and 13C-labelled standards.Food Chemistry, 2009,116:542～554.
72. Guo-Fang Pang ,Yan-Zhong Cao, Jin-Jie Zhang, Chun-Lin Fan, Yong-Ming Liu, Xue-Min Li,et al.Validation study on 660 pesticide residues in animal tissues by gel permeation chromatography cleanup/gas chromatography–mass spectrometry and liquid chromatography–tandem mass spectrometry .Journal of Chromatography A, 2006, 1125:1～30.
73. Gaurav, Varinder Kaur, Ashwini Kumar, Ashok Kumar Malik, P.K.Rai. SPME-HPLC: A new approach to the analysis of explosives. Journal of Hazardous Materials. 2007, 147 691–697.
74. Hao-Yu Shen, Hai-Liang Jiang .Screening, determination and confirmation of chloramphenicol in seafood, meat and honey using ELISA, HPLC–UVD, GC–ECD, GC–MS–EI–SIM and GCMS–NCI–SIM methods. Analytica Chimica Acta, 2005,535:33～41.
75. Jeong-Min Lee, Jin-Won Park, Gi-Chul Jang, Keon-Joong Hwang .Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry.Journal of Chromatography A,2008 (1187):25～33.
76. Jasna Dmitrovic, Siu C. Chan, Sylvia H.Y. Chan. Analysis of pesticides and PCB congeners in serum by GC/MS with SPE sample cleanup.Toxicology Letters 2002(134):253～258.
77. Jeong-Min Lee, Jin-Won Park, Gi-Chul Jang, Keon-Joong Hwang.Comparative study of pesticide multi-residue extraction in tobacco for gas chromatography–triple quadrupole mass spectrometry. Journal of Chromatography A, 2008(1187): 25～33.
78. Koichi Inoue, Shiho Murayama, Kazue Takeba,Yoshihiro Yoshimura, Hiroyuki Nakazawa.Contamination of xenoestrogens bisphenol A and F in honey:safety assessment and analytical method of these compounds in honey.Journal of Food Composition and Analysis, 2003(16):497～506.
79. Liyan Liao,Ji Yang,Yalin Wang, Tonghua Sun,Jinping Jia.Study on a novel circulating cooling solid-phase microextraction method. Journal of Chromatography A,2006,1135:1～5.
80. Li-Fei Wang, Joo-Yeon Lee , Jin-Oh Chung, Joo-Hyun Baik,Sung So, Seung-Kook Park.Discrimination of teas with different degrees of fermentation by SPME–GC analysis of the characteristic volatile flavour compounds.Food Chemistry,2008,(109):196～206.
81. Liu Junting, Cheng Peng1, O. Suzuki .Solid-phase microextraction (SPME) of drugs and poisons from biological samples.Forensic Science International, 1998,97:93～100.
82. Lehotay S J, Kok A, Hiemstra M, et al. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectro-metric detection. J of AOAC Int, 2005, 88(2): 595～614.
83. Min Liu, Yuki Hashi, Yuanyuan Song, Jin-Ming Lin.Simultaneousdetermination of carbamate and organophosphorus pesticides in fruits and vegetables by liquid chromatography–mass spectrometry.Journal of Chromatography A, 2005(1097):183～187.Ion of the chemical composition and
84. Marina Radi?ic′, Svetlana Grujic′, Tatjana Vasiljevic′, Mila Lau?evic .Determination of selected pesticides in fruit juices by matrix solid-phase dispersion and liquid chromatography–tandem mass spectrometry.Food Chemistry2009, 113:712～719.
85. M M Aguilera-Luiz, Jose Luis Martínez Vidal, Roberto Romero-González. Multi-residue determination of veterinary drugs in milk by ultra-high-pressure liquid chromatography–tandem mass spectrometry.Journal of Chromatography A, 2008, 1205:10～16.
86. P.C. Abhilash, Vandana Singh, Nandita Singh.Simplified determination of combined residues of lindane and other HCH isomers in vegetables, fruits, wheat, pulses and medicinal plants by matrix solid-phase dispersion (MSPD) followed by GC–ECD.Food Chemistry, 2009, (113):267～271.
87. Paula Payá,Michelangelo Anastassiades,Dorothea Mack,et al. Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection. Anal Bioanal Chem, 2007, 389:1697～1714.
88. QuEChERS:A mini-multiresidue method for the analysis of pesticides residue in low-fat products.retrieved from www. QuEChERS.com, 2009.
89. Ronald E.Majors. QuEChERS-A New Technique for Multiresidue Analysis of Pesticides in Foods and Agricultural Samples.LC-GC Asia Pacific,2008,11(1):22～31.
90. Robert Loos,Giovanni Locoro, Serafino Contini .Occurrence of polar organic contaminants in the dissolved water phase of the Danube River and its major tributaries using SPE-LC-MS2 analysis .Water Research, 2010, 44(7):2325～2335.
91. Raquel Andrade,Felix G.R. Reyes, Susanne Rath.A method for the determination of volatile N-nitrosamines in food by HS-SPME-GC-TEA.Food Chemistry, 2005,(91):173～179.
92. Steven A.Barker.Applications of matrix solid-phase dispersion in food analysis. Journal of Chromatography A,2000,880:63～68.
93. Schenck, F J, Brown A N, Podhorniak L V, Parker A, Reliford M, Wong J W. A rapid multiresidue method for determination of pesticides in fruits and vegetables by using Acetonitrile Extraction/Partitioning and solid phage extraction column Clean-up. J.AOAC Int,2008,91 (2):422～438.
94. Szilard Szilagyi,Beatriz de la Calle.Development and validation of an analytical method for the determination of semicarbazide in fresh egg and in egg powder based on the use of liquid chromatography tandem mass spectrometry.Analytica Chimica Acta, 2006,572:113～120.
95. The novel radical scavenger IAC is effective in preventing and protecting against post-ischemic brain damage in Mongolian gerbils Donatella Canistro, Alessandra A. Affatato, Antonio Soleti, Vincenzo Mollace, Carolina Muscoli, Francesca Sculco, et al. Journal of the Neurological Sciences 2010(290):90～95.
96. Thanh Dong Nguyen, Ji Eun Yu, Dae Myung Lee, Gae-Ho Lee. A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry.Food Chemistry, 2008, (110):207～213.
97. Thierry Dagnac, Maria Garcia-Chao, Paula Pulleiro, Carmen Garc solid-phase extraction followed by liquid chromatography–tandemmass spectrometry for the multi-residue analysis of pesticides in raw bovine milk.Journal of Chromatography A, 2009,1216:3702～3709.
98. Tomas Cajka, Jana Hajslova, Ondrej Lacina. Rapid analysis of multiple pesticide residues in fruit-based baby food using programmed temperature vaporizer injection–low-pressure gas chromatography–high-resolution time-of-flight mass spectrometry. Journal of Chromatography A, 2008, 1186: 281～294.
99. Vimal K, Balakrishnan, Ken A. Terry John Toito.Determination of sulfonamide antibiotics in wastewater: A comparison of solid phase microextraction and solid phase extraction methods.Journal of Chromatography A, 2006, 1131, 1～10.
100. XU Dun-ming,YANG Fang,LU Sheng-yu, LAN Jin-chang,YU Kong-jie,CAI Chun-ping,et al.Determination of Indoxacarb Residue in Foodstuffs of Plant and Animal Origin by GC-ECD and LC-MS/MS.Agricultural Sciences in China,2008, 7(10):1228～1234.
101. yagiie C ,bayarri S,lazaro R,conchello P,Arino,Herrera A. J.AOAC Int.2001,84:1561.
102. Zsuzsanna Kuklenyik, Xavier A. Bryant, Larry L, Needham, Antonia M. Calafat.SPE/SPME–GC/MS approach for measuring musk compounds in serum and breast milk.Journal of Chromatography B, 2007,858:177～183.
103. ZENG Dong-ping, LIN Cui-ping, ZENG Zhen-ling, HUANG Xian-hui and HE Li-min.Multi-Residue Determination of Eight Anabolic Steroids by GC-MS in Muscle Tissues from Pigs. Agricultural Sciences in China, 2010, 9(2): 306-312.ia-Jares, Maria Llompart Dispersive.
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