固相萃取/液质联用测定竹笋中丁烯氟虫腈农药残留研究  

Determination of Butylene Fipronil Residue in Bamboo Shoots by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：丁明[1,2] 钟冬莲[1] 汤富彬[1] 方伟[2] 

机构地区：[1]中国林业科学研究院亚热带林业研究所,浙江富阳311400 [2]浙江农林大学林业生物技术学院,浙江临安311300

出　　处：《分析测试学报》2013年第3期372-376,共5页Journal of Instrumental Analysis

基　　金：林业公益性行业科研专项经费(201204414)

摘　　要：建立了高效液相色谱-串联质谱(HPLC-MS/MS)测定竹笋中丁烯氟虫腈残留的分析方法。样品采用乙腈提取,经PSA固相萃取小柱净化后,采用Waters Atlantis T3色谱柱(2.1 mm×150 mm×5μm),以含5mmol/L乙酸铵的0.1%甲酸水溶液和乙腈为流动相梯度洗脱,电喷雾离子源负离子模式多反应监测(MRM)模式定性分析,以氟虫腈为内标物质内标法消除基质效应定量测定丁烯氟虫腈。该方法在5.0～100.0μg/L范围内具有良好的线性关系,相关系数大于0.994 8;4、8、32μg/kg 3个加标水平下的平均回收率为76%～103%,相对标准偏差(RSDs)为3.2%～9.9%;方法的检出限(信噪比S/N=3)和定量下限(S/N=10)分别为0.21μg/kg和0.69μg/kg。该方法较气相色谱法和气相色谱质谱联用法具有更高的准确性和灵敏度,且更加简单快速,可满足竹笋中丁烯氟虫腈农药残留的检测要求。A simple and efficient method based on solid phase extraction （SPE） cartridge and liquid chromatography-tandem mass spectrometry （LC - MS/MS） was developed for the determination of butylene fipronil residue in bamboo shoots. Samples were extracted with acetonitrile, and the extract was purified with PSA SPE column. The detection of butylene fipronil was performed by LC - MS/MS under multiple reaction - monitoring mode （MRM）. Butylene fipronil could be completely separated in 15 min with an excellent linear relationship in the range of 5.0 - 100. 0 μg/L. The detection limit （ S/N =3 ） and quantitation limit for butylene fipronil were 0.21 μg/kg and 0.69 μg/kg, respectively. The recoveries of butylene fipronil at three spiked levels of 4, 8, 32. μg · kg^-1 were in the range of 76% - 103% with relative standard deviations of 3.2% -9.9%. Compared with GC and GC - MS method, the proposed method was rapid, sensitive and accurate, and could meet the requirement for the determination of butylene fipronil residue in bamboo shoots.

关 键 词：高效液相色谱-串联质谱 丁烯氟虫腈 竹笋 残留 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]