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| Effects of Four Kinds of Purification Methods for Determination of 19 Pesticide Residues in Substrates of Different Pigments Analyzed by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:UPLC-MS/MS solid phase extraction dispersive solid phase extraction pigment pesticide residues |
| Author | Institution |
| YAN Zhen,NIE Ji-yun,XU Guo-feng,LI Hai-fei,LI Jing,LI Zhi-xia,WU Yong-long,KUANG Li-xue |
中国农业科学院果树研究所，农业部果品质量安全风险评估实验室（兴城），农业部果品及苗木质量监督检验测试中心（兴城） |
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| Abstract: |
| 19 pesticide residues in substrates of different pigments including apple,tomato,ginger and leek,were determined by UPLC-MS/MS.Through comparing four kinds of purification methods,the best detection method was selected.The samples were purified by solid phase extraction（SPE） and dispersed solid phase extraction（QuEChERS）.The SPE columns included TPS column,PC/NH2 column and NH2 column.The absorbent of QuEChERS was the mixture of PSA（N-Propyl ethylenediamine） and C18.The detection was performed in multiple reaction monitoring mode,and quantified by the external standard method．The results indicated that the calibration curves of 19 pesticides were linear in the range of 5-100 μg/kg with correlation coefficients more then 0.99．The adsorption effect of TPS column on pigment is best,while the worst one is PSA+C18.The average recoveries for all pesticides in the four substrates purified with TPS column,NH2 column and PSA+C18 were in the range of 72%-107%,71%-110% and 72%-108%,respectively.The recoveries of carbendazim in gingers and leek purified with PC/NH2 column were very low,while those were even zero in apples and tomatoes.The recoveries of the other 18 pesticides were in the range of 71%-110%.The RSDs of phoxim were generally higher than the others,and those of the other pesticides were less than 20% after cleaned up with TPS column,PC/NH2 column,NH2 column and PSA+C18.The limits of detection（LOD ） were in the range of 0.001-3,0.007-3,0.02-4 and 0.02-2 μg/kg for 19 pesticides,with limits of quantitation（LOQ） of 0.003-10，0.02-10，0.06-15 and 0.05-8 μg/kg,respectively.The study provided a reliable basis for accurate,efficient and economical detection of targeted analytes. |
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