超高效液相色谱-串联质谱法对比4种净化方式对不同色素含量基质中1怨种农药残留检测的影响

摘要

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 meth-ods,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 5-100μg/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 recover-ies 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,effi-cient and economical detection of targeted analytes.%采用超高效液相色谱-串联质谱仪（ UPLC-MS/MS）对含有不同色素等干扰物的4种基质（韭菜、姜、番茄和苹果）中19种农药残留进行检测，对比了4种净化方式对检测结果的影响，筛选出最佳检测方法。试样采用固相萃取法（ SPE）和分散固相萃取法（ QuEChERS）进行前处理净化。固相萃取柱包括3种，TPS柱、PC/NH2柱（石墨化碳黑氨基柱）和NH2柱（氨基柱），分散固相萃取的吸附剂为PSA（ N-丙基乙二胺）和C18混合剂，外标法定量。研究表明，19种农药在5~100μg/kg质量浓度范围内线性关系良好，相关系数均大于0.99；TPS柱对色素的吸附效果最好，PSA+C18的吸附效果最差；经TPS柱、NH2柱和PSA+C18净化过的4种基质中，19种农药的平均加标回收率分别为72％~107％，71％~110％和72％~108％；经PC/NH2柱净化过的韭菜和姜中，多菌灵的回收率很低，番茄和苹果中无回收，其他18种农药的加标回收率为71％~110％；经TPS柱、PC/NH2柱、NH2柱和PSA+C18净化后，辛硫磷的相对标准偏差（ RSD）普遍较高，其他18种农药的RSD值均小于20％，19种农药的检出限分别为0.001~3，0.007~3，0.02~4，0.02~2μg/kg，定量下限分别为0.003~10，0.02~10，0.06~15，0.05~8μg/kg。本研究为准确、高效、经济的检测目标物提供了可靠依据。