基质分散固相萃取和超高效液相色谱-串联质谱法测定水果、蔬菜中的11种杀菌剂  

Determination of 11 fungicides in fruits and vegetables by matrix dispersive solid phase extraction and UPLC-MS/MS method

作　　者：廖艳华[1] 唐阳 周劭桓[1] 林文斯[1] 周能志 陈杰[1] 梁川[1] LIAO Yan - hua, TANG Yang, ZHOU Shao - huan, LIN Wen - shi, ZHOU Neng - zhi, CHEN Jie, LIANG Chuan Guangxi(Center for Disease Control and Prevention, Nanning , Guangxi 530028, Chin)

机构地区：[1]广西壮族自治区疾病预防控制中心,广西南宁530028

出　　处：《现代预防医学》2018年第7期1268-1273,共6页Modern Preventive Medicine

基　　金：广西壮族自治区卫生和计划生育委员会科研课题"广西各色水果中乙烯利留量的调查研究"(Z2012035)

摘　　要：目的建立水果、蔬菜中11种杀菌剂的基质分散固相萃取-液相色谱-串联质谱分析方法。方法样品中的杀菌剂经乙腈提取,以PSA、石墨化炭黑和C18为吸附剂的基质分散固相萃取净化,最后用C18柱分离,以乙腈和0.05%甲酸水为流动相,经电喷雾离子源(ESI+)电离,多反应监测(MRM)模式串联质谱检测。结果腐霉利的检测线性范围为10~500ng/ml,检出限为10μg/kg,其余10种杀菌剂的检测线性范围1.0~50ng/ml,检出限为1μg/kg;11中杀菌剂的平均加标回收率在80.3%~115.6%之间,相对标准偏差在3.9%~11.2%之间。结论该方法前处理简单、快速、有效、准确灵敏、稳定和安全,适合于水果蔬菜中11种杀菌剂的检测。Objective To develop a method for determination of 11 fungicide residues in fruits and vegetables by matrix dispersive solid phase extraction and UPLC - MS/MS. Methods The fungicides in fruits and vegetables were extracted with acetonitrile, purified with matrix dispersive solid phase extraction using PSA, GCB and C18 as adsorbents. The sample solution was separated on PhenomenexC18 （150mm×3.0mm, size 1.7 μm ） with gradient elution using aeetronitrile -0.05% formic acid as mobile phase and detected by MS/MS using positive electrospray ionization （ ESI ＋ ） under the multiple reaction monitoring（MRM）. Results The linear range of proeymidone was 10 -500ng,/ml with the limit of detection （LOD） of 10μg/ kg. The linear ranges of other ten fungicide were 1.0× 50ng/ml and all the LODs were 1 μg/kg. The average recoveries were in the range of 80.3% - 115.6%, with relative standard deviations （ RSD ） of 3.9% - 11.2%. Conclusion The method is simple, time -saving, accurate and sensitive. It is suitable for detection of 11 fungicides residue in fruits and vegetables.

关 键 词：超高效液相色谱-串联质谱 基质分散固相萃取 杀菌剂 水果 蔬菜 

分 类 号：R115[医药卫生—公共卫生与预防医学]