CAJ | 학술논문

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。
채용초고효액상색보-천련질보의（ UPLC-MS/MS）대함유불동색소등간우물적4충기질（구채、강、번가화평과）중19충농약잔류진행검측，대비료4충정화방식대검측결과적영향，사선출최가검측방법。시양채용고상췌취법（ SPE）화분산고상췌취법（ QuEChERS）진행전처리정화。고상췌취주포괄3충，TPS주、PC/NH2주（석묵화탄흑안기주）화NH2주（안기주），분산고상췌취적흡부제위PSA（ N-병기을이알）화C18혼합제，외표법정량。연구표명，19충농약재5~100μg/kg질량농도범위내선성관계량호，상관계수균대우0.99；TPS주대색소적흡부효과최호，PSA+C18적흡부효과최차；경TPS주、NH2주화PSA+C18정화과적4충기질중，19충농약적평균가표회수솔분별위72％~107％，71％~110％화72％~108％；경PC/NH2주정화과적구채화강중，다균령적회수솔흔저，번가화평과중무회수，기타18충농약적가표회수솔위71％~110％；경TPS주、PC/NH2주、NH2주화PSA+C18정화후，신류린적상대표준편차（ RSD）보편교고，기타18충농약적RSD치균소우20％，19충농약적검출한분별위0.001~3，0.007~3，0.02~4，0.02~2μg/kg，정량하한분별위0.003~10，0.02~10，0.06~15，0.05~8μg/kg。본연구위준학、고효、경제적검측목표물제공료가고의거。
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.