氣相串聯質譜儀檢測杭菊多重農藥殘留技術之評估

Analysis Pesticides Residues in Chrysanthemum Flowersby Gas Chromatography with Triple Quadrupole Mass Spectrometer

陳裕文(Yu-wun Chen) ； 巫嘉昌(Chia-Chang Wu) ； 侯金日(Chin-Jin Hou)

《嘉大農林學報》 12卷2期 (2015/09) Pp. 13-38

摘要

本研究昌在建立杭菊中殘留農藥之氣相串聯質譜儀檢測技術，杭菊樣品以乙腈（acetonitrile）進行液－液萃取（liquid-liquid extraction, LLE）及以矽酸鎂固相萃取匣進行固相萃取（solid phase extraction, SPE）後，搭配氣相層析串聯質譜儀（gas chromatography/triple quadrupole mass spectrometer, GC/MS/MS）建立杭菊乾花中112種之多重農藥殘留分析方法。結果顯示，所有農藥皆其有良好的線性關條（R^2≧0.995）。在農藥最低檢測控限（limit of detection, LOD）和最低定量極限（limit of quantitation, LOQ）部分，112種農藥在GC/MS/MS中測定的LOD≦10μg/kg，有79.46%的農藥之LOQ為10μg/kg。在添加高濃度農藥（50和100μg/kg）回收率介於70%-120%分別達77.68%和88.39%'而在添加低濃度農藥（10和20μg/kg）下，則不到10%的農藥達到此標準。顯示本研究所建立之分析方法，可應用於國內外杭菊產銷之監測檢驗。

關鍵字

杭菊 ； 液－液萃取法 ； 固相萃取法 ； 氣相層析串聯質譜儀 ； 多重農藥殘留 ； 覆滅螨

並列摘要

In this study, the 112 multiple pesticide residues in Chrysanthemum morifolium were extracted by LLE with acetonitrile as the solvent followed by sample clean-up by SPE using florisil cartridges, and the extracts were analyzed by GC/MS/MS. The present results showed good linearity by correlation coefficients of more than 0.995 for all analyses. The LOD of all analyses were less or equal to 10 μg/kg. The LOQ were 10 μg/kg for approximately 79.46% of pesticides. The attained recoveries were typically between 70% and 120% with the RSD values typically lower than 20% were 77.68% and 88.39% of pesticides at spiking levels of 50 and 100μg/kg. Then, at spiking levels of 10 and 20μg/kg, there were below 10% of pesticides reaching the standard. The results demonstrated that the GC/MS/MS method was successfully utilized to determine the trace level amounts of pesticides residues in Chrysanthemum flowers samples.

並列關鍵字

Chrysanthemum flower ； liquid-liquid extraction ； solid phase extraction ； C/MS/MS ； multiple pesticide residues