色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2015年
8期
869-877
,共9页
刘小勤%佟玲%孟文婷%孙国祥
劉小勤%佟玲%孟文婷%孫國祥
류소근%동령%맹문정%손국상
固相萃取%气相色谱-三重四极杆质谱%农药残留%白芍
固相萃取%氣相色譜-三重四極桿質譜%農藥殘留%白芍
고상췌취%기상색보-삼중사겁간질보%농약잔류%백작
solid-phase extraction( SPE)%gas chromatography-triple quadrupole tandem mass spectrometry( GC-QqQ-MS)%pesticide residues%Paeoniae Radix Alba
采用固相萃取技术( SPE)结合气相色谱-三重四极杆质谱( GC-MS/MS)建立了白芍中99种农药同时检测的分析方法。试样用乙酸乙酯提取,采用氨基固相萃取柱净化后,在 GC-MS/MS 多反应监测( MRM)模式下进行检测,基质匹配标准曲线内标法定量。结果表明,99种农药在0.001~0.25 mg/L 范围内线性关系良好,相关系数( r2)大于0.99,方法定量限为0.001~0.050 mg/kg。加标水平为0.05、0.10和0.20 mg/kg时,99种农药的平均回收率为66.7%~128.0%,相对标准偏差( RSD,n=6)小于18.3%。对市售的13批样品进行测定,其中4批样品中检出微量的毒死蜱和 p,p′-滴滴伊。实验证明,建立的 SPE净化和 GC-QqQ-MS相结合的检测方法具有准确可靠、灵敏度高等优点,适用于白芍中多农药残留的同时筛查测定。
採用固相萃取技術( SPE)結閤氣相色譜-三重四極桿質譜( GC-MS/MS)建立瞭白芍中99種農藥同時檢測的分析方法。試樣用乙痠乙酯提取,採用氨基固相萃取柱淨化後,在 GC-MS/MS 多反應鑑測( MRM)模式下進行檢測,基質匹配標準麯線內標法定量。結果錶明,99種農藥在0.001~0.25 mg/L 範圍內線性關繫良好,相關繫數( r2)大于0.99,方法定量限為0.001~0.050 mg/kg。加標水平為0.05、0.10和0.20 mg/kg時,99種農藥的平均迴收率為66.7%~128.0%,相對標準偏差( RSD,n=6)小于18.3%。對市售的13批樣品進行測定,其中4批樣品中檢齣微量的毒死蜱和 p,p′-滴滴伊。實驗證明,建立的 SPE淨化和 GC-QqQ-MS相結閤的檢測方法具有準確可靠、靈敏度高等優點,適用于白芍中多農藥殘留的同時篩查測定。
채용고상췌취기술( SPE)결합기상색보-삼중사겁간질보( GC-MS/MS)건립료백작중99충농약동시검측적분석방법。시양용을산을지제취,채용안기고상췌취주정화후,재 GC-MS/MS 다반응감측( MRM)모식하진행검측,기질필배표준곡선내표법정량。결과표명,99충농약재0.001~0.25 mg/L 범위내선성관계량호,상관계수( r2)대우0.99,방법정량한위0.001~0.050 mg/kg。가표수평위0.05、0.10화0.20 mg/kg시,99충농약적평균회수솔위66.7%~128.0%,상대표준편차( RSD,n=6)소우18.3%。대시수적13비양품진행측정,기중4비양품중검출미량적독사비화 p,p′-적적이。실험증명,건립적 SPE정화화 GC-QqQ-MS상결합적검측방법구유준학가고、령민도고등우점,괄용우백작중다농약잔류적동시사사측정。
A method was established for the simultaneous determination of 99 pesticide resi-dues with combination of solid-phase extraction technique ( SPE ) and gas chromatography-triple quadrupole tandem mass spectrometry( GC-QqQ-MS ). The sample was extracted with ethyl acetate,and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring ( MRM ) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0. 001-0. 25 mg/L,with correlation coefficients(r2)> 0. 99. The limits of quantification( LOQs ) were between 0. 001-0. 050 mg/kg. The recoveries were between 66. 7% and 128. 0% with RSD values typically lower than 18. 3% at three spiked levels of 0. 05, 0. 10 and 0. 20 mg/kg. This method has been applied to determine thirteen batches of commer-cially available samples,chlorpyriphos-ethyl and p,p′-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate,reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.