QuEChERS净化—超高效液相色谱--串联质谱法同步测定荔枝中10种植物生长调节剂残留  

Simultaneous determination of ten plant growth regulators residues in litchi by QuEChERS clean up-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：吴学进[1] 刘春华[1] 罗金辉[1] 李春丽[1] 马晨[1] 乐渊[1] 吴南村[1] WU Xue-jin;LIU Chun-hua;LUO Jin-hui;LI Chun-li;MA Chen;LE Yuan;WU Nan-cun(Analysis and Testing Center,Chinese Academy of Tropical Agricultural Sciences/Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Haikou 571101,China)

机构地区：[1]中国热带农业科学院分析测试中心/海南省热带果蔬产品质量安全重点实验室,海口571101

出　　处：《南方农业学报》2020年第10期2532-2539,共8页Journal of Southern Agriculture

基　　金：国家农产品质量安全风险评估重大专项(GJFP2019013);中国热带农业科学院基本科研业务费专项(1630082020009,1630082017001,1630082020002)。

摘　　要：【目的】建立同步测定荔枝中甲哌啶、矮壮素等10种植物生长调节剂(PGRs)残留的QuEChERS净化—超高效液相色谱—串联质谱法(UPLC-MS/MS),为荔枝中多种PGRs残留同步检测提供技术参考。【方法】荔枝样品以1%(v/v)乙酸—乙腈提取,经优化QuEChERS前处理后,净化后的样品提取液以Agilent InfinityLab Poroshell 120 EC-C18柱为分离色谱柱,甲醇—5 mmol/L乙酸铵水溶液(含0.1%甲酸,v/v)缓冲溶液为流动相梯度洗脱,以UPLC-MS/MS在选择反应监测模式下对甲哌啶等10种PGRs目标物残留进行测定。【结果】在5~100μg/kg范围内,10种PGRs质量浓度与对应的峰面积呈良好线性,相关系数(r2)均>0.9950;检出限范围为0.03~0.60μg/kg。在10、25和100μg/kg 3个添加水平范围内,平均回收率在71.8%~109.2%,相对标准偏差(RSD)在0.6%~10.0%。用优化的QuEChERS净化-UPLCMS/MS对40份荔枝样品进行检测,其中1份样品检出多效唑,1份样品检出芸苔素内酯,PGRs检出率为5.0%。【结论】建立的QuEChERS净化-UPLC-MS/MS简便、快速,具有良好的灵敏度、准确度和精密度,可用于同步测定甲哌啶等10种PGR在荔枝中的残留。【Objective】A method for simultaneous determination of ten plant growth regulators(PGRs)residues in litchi,such as meperidine,chlorpromazine and others,was developed by using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)in combination with QuEChERS methodology,to provide reference for simultaneous determination of multiple PGRs residue in litchi.【Method】The litchi samples were extracted with acetonitrile containing 1%(v/v)acetic acid and purified by the optimized QuEChERS pretreatment method,then the purified sample extracting solutions were separated in Agilent InfinityLab Poroshell 120 EC-C18 column with methanol-5 mmol/L ammonium acetate solution(containing 0.1%formic acid,v/v)as mobile phase by gradient program,and analyzed by using UPLC-MS/MS in selective reaction monitoring(SRM)mode for mepiquat chloride and other nine PGRs residues in samples.【Result】The mass concentrations of ten PGRs showed good linearity with the corresponding peak area in the range of 5-100μg/kg,and the correlation coefficient(r2)was more than 0.9950.The limits of detection(LODs)ranged from 0.03 to 0.60μg/kg.The average recoveries at three spiked levels of 10,25,100μg/kg for all target compounds in the samples were in the range of 71.8%-109.2%,with relative standard deviations(RSD)between 0.6%and 10.0%.The optimized UPLC-MS/MS in combination with QuEChERS methodology mention above was used to detect 40 litchi samples,paclobutrazol was detected in one sample and so was brassinolide,the detection rate of PGRs was 5.0%.【Conclusion】The QuEChERS purofied-UPLC-MS/MS method is simple,rapid with high sensitivity and good repeatability,accuracy and precision,which can be used for simultaneous determination of ten PGR residues above mentioned in litchi.

关 键 词：荔枝 QUECHERS 植物生长调节剂(PGRs) 超高效液相色谱—串联质谱(UPLC-MS/MS) 

分 类 号：S482.8[农业科学—农药学]