加速溶剂萃取-气相色谱/质谱法同时测定土壤中拟除虫菊酯类等18种农药残留

李俊; 肖雅雯; 王震; 赵为武

加速溶剂萃取-气相色谱/质谱法同时测定土壤中拟除虫菊酯类等18种农药残留

1.
贵州省农产品质量安全监督检验测试中心, 贵州贵阳 550004
2.
华南农业大学资源环境学院, 广东广州 510642
3.
贵州省农产品质量安全监督检验测试中心, 贵州贵阳 550004
4.
贵州省农产品质量安全监督检验测试中心, 贵州贵阳 550004

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出版历程
- 收稿日期: 2010-12-13
- 修回日期: 2011-03-16

Simultaneous Determination of 18 Pesticide Residues including Pyrethroids in Soils by Gas Chromatography-Mass Spectrometry with Accelerated Solvent Extraction

1.
Supervision and Testing Center for Agri-Produce Quality and Safety of Guizhou Province, Guiyang 550004, China
2.
College of Natural Resources and Environment, South China Agricultural University, Guangzhou 510642, China
3.
Supervision and Testing Center for Agri-Produce Quality and Safety of Guizhou Province, Guiyang 550004, China
4.
Supervision and Testing Center for Agri-Produce Quality and Safety of Guizhou Province, Guiyang 550004, China

摘要

摘要: 采用正己烷-丙酮-磷酸混合溶剂为提取剂,在萃取温度100℃ 、压力10.3 MPa条件下,用快速溶剂萃取仪提取土壤样品,石墨碳黑氨基固相萃取柱净化,PTV大体积进样,气相色谱-质谱联法同时检测六六六(HCHs)、滴滴涕(DDTs)和10种拟除虫菊酯类农药(联苯菊酯、甲氰菊酯、氯氟氰菊酯、氯菊酯、氯氰菊酯、氟氯氰菊酯、氟氨氰菊酯、氰戊菊酯、氟氰戊菊酯、溴氰菊酯)共18种农药残留。在10~20 μg/kg的添加浓度下,目标化合物平均回收率为82.84%~96.33%,相对标准偏差(RSD,n=6)为3.21%~7.34%;在20~40 μg/kg的添加浓度下,目标化合物平均回收率为80.55%~103.76%,RSD(n=6)为2.56%~5.78%;在40~80 μg/kg的添加浓度下,目标化合物平均回收率81.56%~95.38%,RSD(n=6)为2.19%~5.88%。方法检出限为0.11~3.40 μg/kg,实际样品检测的RSD(n=3)为4.94%~8.74%。方法简单快速、灵敏度高、准确度好,可以满足土壤中HCHs、DDTs和拟除虫菊酯类农药残留的实际检测需要。
- 土壤 /
- 拟除虫菊酯类 /
- 六六六 /
- 滴滴涕 /
- 快速溶剂萃取 /
- 气相色谱-质谱法
Abstract: A method was developed for simultaneous determination of 18 pesticide residues in soils, including hexachlorocyclohexanes (HCHs), dichlorodiphenyltrichloroethanes (DDTs) and other 10 kinds of pyrethroid. The soil samples were distilled with Accelerated Solvent Extraction (ASE) and extracted by hexane-acetone-H₃PO₄ at extraction temperature of 100℃ and pressure of 10.3 MPa. The distilled solutions were purified by solid phase extraction (SPE). The purified solutions were injected into Gas Chromatography-Mass Spectrometry (GC-MS) by using programmed temperature vaporization (PTV) and large volume injector (LVI). If the spiked level was 10-20 μg/kg, the recoveries of target compounds were 80.55%-96.33% and the relative standard deviations (RSDs, n=6) were 3.21%-7.34%. If the spiked level was 20-40 μg/kg, the recoveries were 80.55%-103.76% and RSDs (n=6) were 2.56%-5.78%. If the spiked level was 40-80 μg/kg, the recoveries were 81.56%-95.38%, RSDs(n=6) were 2.19%-5.88%. The method detection limits were 0.11-2.38 μg/kg, RSDs (n=3) were 4.94%-8.74% for real samples. The method is simple and rapid with high sensitivity making it suitable for simultaneous determination of residues of benzex and DDTs and pyrethroid in soils.
- soil /
- pyrethroids /
- hexachlorocyclohexanes /
- (HCHs) /
- dichlorodiphenyltrichloroethanes /
- (DDTs)

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参考文献(24)

华纯.拟除虫菊酯类农药的进展和剂型[J].世界农药,2009,31(5):39-44.

Serrano R, Barreda M, Pitarch E, Hernandez F. Determination of low concentrations of organochlorine pesticides and PCBs in fish feed and fish issues from aquaculture activities by gas chromatography with tandem mass spectrometry[J]. Journal of Separation Science, 2003, 26:75-86.

王玲玲,王潇磊,南淑清,焦飞,邢核,李国刚.ASE提取土壤中有机氯农药的方法研究[J].中国环境监测, 2006, 22(5):19-22.

EPA Method 8081A.Organochlorine pesticides by gas chromatography [S].

于彦彬,谭培功,王孝钢,万述伟.毛细管柱气相色谱法测定土壤中的有机氯农药[J].分析试验室,2004,23(7):47-50.

刘文长,陶文靖,程丽娅,余兴,田旻,黄勤,李胜生.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[J].岩矿测试,2009,24(6):541-544.

陈卫明,邓天龙,张勤,李庆霞.土壤中有机氯农药残留的分析技术研究进展[J].岩矿测试,2009,28(2):151-156.

佟玲,吴淑琪,杨佳佳,张玲金.土壤中25种有机氯农药和多氯联苯的气相色谱分析方法研究[J].岩矿测试,2010,29(3):277-281.

宋淑玲,饶竹,赵威,李松.地质调查样品中有机氯农药分析存在的困难和解决方法[J].岩矿测试,2010,29(3):271-276.

薛佳.固相小柱萃取法测定多目标生态地球化学评价土壤样品中有机氯农药含量[J].福建分析测试,2008,17(3):49-52.

柳丽丽,陈莎,任仁.有机氯农药的固相萃取前处理技术和分析方法[J].北京工业大学学报,2003,29(1):74-78.

Saito K, Takekuma M, Ogawa M, Kobayashi S, Sugawara Y, Lshizuka M, Nakazawa H, Matsuki Y. Extraction and cleanup methods of dioxins in house dust from two cities in Japan using ASE and a disposable multilayer silica-gel cartridge[J].Chemosphere,2003, 53:137-142.

郜红建,蒋新,常江,张自立.加速溶剂提取-气相色谱法测定蔬菜中的有机氯农药[J].生态环境,2007,16(1):50-53.

Banjoo D R, Nelson P K.Imaroved ultrasonic extraction procedure for the determination of polycyclic aromatic hydrocarbons in sediments[J].Jourmal of Chrmatography A,2005,1066(1-2):9-18.

Klanova J, Matyiewiczova N, Macka Z, Prosek P, Laska K, Klan P. Persistent organic pollutants in soils and sediments from James Ross Island, Antarctica[J].Environmental Pollution,2008,152:416-423.

EPA Method 3545, Pressurized fluid extraction (PEE)[S].

Hu B Z, Song W H, Xie L P, Shao T F. Determination of 33 pesticides in tea using accelerated solvent extraction/gel permeation chromatography and solid phase extraction/gas chromatography-mass spectrometry[J].Chinese Journal of Chromatography,2008,26(1):22-28.

饶竹,何淼,陈巍,李松,刘艳.土壤样品中有机磷农药的加速溶剂萃取-气相色谱测定[J].岩矿测试,2010,29(5):503-507.

张岩,张景发,陈艳梅,孟娟,韩翠英.加速溶剂萃取-气相色谱法测定土壤中有机氯农药和多氯联苯[J].岩矿测试,2010,29(5):491-496.

汪瑾彦,汤桦,陈大舟,吴雪,冯洁,吴学丽,李蕾.气相色谱-质谱法同时测定河流沉积物中多环芳烃和有机氯农药[J].岩矿测试,2010,29(3):225-230.

李庆霞,刘亚轩,陈卫明,张勤.微波萃取-气相色谱/气相色谱-质谱法测定土壤中18种有机氯农药[J].岩矿测试,2010,29(2):118-122.

黄园英,佟玲,张玲金,吴淑琪,汪雨.ASE提取和GPC净化气相色谱法快速测定土壤中痕量有机氯代化合物[J].生态环境,2008,17(1):184-189.

龚钟明,曹军,朱雪梅,崔艳红,郭丽青,陶澍,沈伟然,赵喜梅,韩兰香.天津市郊污灌区农田土壤中的有机氯农药残留[J].农业环境保护,2002,21(5):459-461.

郭永泽,刘磊,张玉婷,李辉,邵辉,李娜. 大体积进样/气相色谱技术在农药残留分析中的应用[J].天津农业科学,2010,161(4):30-36.