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《化学分析计量》 2017年第01期
DOI:10.3969/j.issn.1008-6145.2017.01.008
QuEChERS前处理联合UPLC-MS/MS法检测花生中22种农药残留
李婵君,王毅红,王彦超,董素静,段鹿梅
郑州市农产品质量检测流通中心 
Determination of 22 Pesticide Residues in Peanut by QuEChERS-UPLC-MS/MS
李婵君,王毅红,王彦超,董素静,段鹿梅
Zhengzhou Testing Center for Quality of Agricultural Products, Zhengzhou 450006, China 
摘要:建立了QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)前处理联合UPLC-MS/MS法检测花生中22种农药残留的方法。样品用10 mL乙腈提取,以多壁碳纳米管、N-丙基乙二胺为吸附剂,对2 mL提取液进行净化,净化液稀释至2倍体积,以MRM扫描方式、正负离子模式同时分析。22种农药在10,20,50 μg/kg 3个添加水平下,平均回收率为70.6%~121.2%,相对标准偏差小于10%(n=6);多菌灵、抗蚜威、扑草净在0.05~10μg/L,啶虫脒、氟虫腈砜、苯醚甲环唑、哒螨灵、嘧霉胺、嘧菌酯在0.5~20 μg/L,烯酰吗啉、噻虫嗪、氟啶脲、灭幼脲、吡虫啉、甲维盐、除虫脲、氟虫腈、氟甲腈、氟虫腈亚砜、咪鲜胺、二甲戊灵在0.5~50 μg/L之间,阿维菌素在0.5~100 μg/L范围内线性良好,相关系数r2均大于0.9950。22种农药的定量限在2 μg/kg以下,远低于各待测农药最高残留限量标准(MRL)。该法适于花生中农药残留的同时快速检测。 
Abstract:QuEChERS-UPLC-MS/MS was proposed for determination of 22 pesticide residues in peanut. The sample was extracted with 10 mL acetonitrile. 2 mL of the supernatant was taken and cleaned up with multi-walled carbon nanotubes (MWCNTs) and PSA. After being diluted to 2 times volume, the purified solution was determined by UPLC-MS/MS under the mode of MRM. ESI was adopted in MS operated in the positive negative ion switch mode. Recovery rates at the three concentrations of 10, 20, 50 μg/kg ranged from 70.6% to 121.2% with RSDs less than 10%(n=6). Linear relationships between values of peak area and mass concentration were found in the range of 0.05-10 μg/L for carbendazim, pirimicarb and prometryne, 0.5-20 μg/L for acetamiprid, fipronil-sulfone, difenocoazole, pyridaben, pyrimethanil and azoxystrobin, 0.5-50 μg/L for dimethomorph, thiamethoxam, chlorfluazuron, chlorbenzuron, imidacloprid, emamectin benzoate, diflubenzuron, fipronil, fipronil-desulfinyl, fipronil-sulfide, prochloraz and pendimethalin, and 0.5-100 μg/L for abamectin, with the linear relative coefficients (r2) more than 0.9950. The LOQs of 22 pesticide residues were less than 2 μg/kg, which were significantly lower than the respective MRLs. This method can be used in the determination of 22 pesticide residues in peanut. 
关键词:QuEChERS;超高液相串联质谱法;花生;农药残留 
Keywords:QuEChERS; UPLC-MS/MS; peanut; pesticide residues 
本文引用格式:
李婵君,王毅红,王彦超,等.QuEChERS前处理联合UPLC-MS/MS法检测花生中22种农药残留[J].化学分析计量,2017,26(1):33-37.
LI C J,WANG Y H,WANG Y C,et al.Determination of 22 Pesticide Residues in Peanut by QuEChERS-UPLC-MS/MS[J]. Chemical analysis and meterage,2017,26(1):33-37. 

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