超高效液相色谱-串联质谱法测定果蔬中6种植物生长调节剂残留及其污染水平分析  

Determination of residues of six plant growth regulators in fruits and vegetables by ultra high performance liquid chromatography-tandem mass spectrometry and analysis of their pollution levels

作　　者：肖国军[1] 许桂锋[1] 李波[1] 王生[1] 蔡超海[1] 覃玲[1] XIAO Guo-jun;XU Gui-feng;LI Bo;WANG Sheng;CAI Chao-hai;QIN Ling(Maoming Center for Disease Control and Prevention,Maoming,Guangdong 525000,China)

机构地区：[1]茂名市疾病预防控制中心

出　　处：《实用预防医学》2019年第9期1034-1039,共6页Practical Preventive Medicine

基　　金：茂名市科技计划项目(项目编号:2018296)

摘　　要：目的建立果蔬中常见植物生长调节剂赤霉素、噻苯隆、4-氯苯氧乙酸(4-chlorophenoxyacetic acid,4-CPA)、氯吡脲、2,4-二氯苯氧乙酸(2,4-dichlorophenoxyacetic acid,2,4-D)、多效唑残留的超高效液相色谱-串联质谱法,对市售水果和蔬菜中常见植物生长调节剂残留进行污染水平分析。方法用1%乙酸乙腈超声提取样品中的植物生长调节剂,高速离心后,提取液经QuEChERS净化管净化,过0.22μm滤膜,经Shim-pack XR-ODS C18(2.0 mm×75 mm,2.2μm)色谱柱分离,以乙腈-0.1%甲酸水做流动相,梯度洗脱,采用电喷雾离子源正负离子检测模式(ESI±)和多重反应监测模式测定,基质匹配标准曲线,内标法定量。结果在果蔬基质中,该方法在1.0~200μg/L内相关系数均>0.999,回收率为91.1%~108.0%,相对标准偏差(RSD)为0.3%~4.5%,检出限为0.01~1.0μg/kg,定量限为0.03~3.0μg/kg。结论该方法操作简便、准确、快速、检出限低、重现性好,适用于果蔬中常见植物生长调节剂残留的检测。Objective To establish a method for the determination of gibberellin, thidiazuron, 4-chlorophenoxyacetic acid(4-CPA), chlorfenuron, 2,4-dichlorophenoxyacetic acid(2,4-D) and paclobutrazol residues in fruits and vegetables by ultra high performance liquid chromatography-tandem mass spectrometry, and to analyze the pollution levels of common plant growth regulator residues in marketed fruits and vegetables. Methods The plant growth regulators were extracted with 1% acetonitrile acetatevortex ultrasound. After high speed centrifugation,the extract was purified by Qu ECh ERS purification tube,filtered through a0.22 um filter membrane and separated by Shim-pack XR-ODS C18( 2.0 mm × 75 mm,2.2 μm) chromatography column. Acetonitrile-0.1% formate water was used as a mobile phase. Gradient elution was performed by electrospray ion source positive and negative ion detection mode( ESI±) and multiple reaction monitoring( MRM) mode,and matrix-matched internal standard method was applied to quantify the plant growth regulator residues. Results In the fruit and vegetable substrate,the method had good linearities in the range of 1.0 μg/L-200 μg/L,with the correlation coefficients of greater than 0.999. The recovery rates of the method were 91. 1%-108. 0%,with the relative standard deviations( RSDs) of 0. 3%-4. 5%. The limits were 0. 01 μg/kg-1.0 μg/kg,and the limits of quantification were 0.03 μg/kg-3.0 μg/kg. Conclusions The method is simple,accurate and rapid,with low detection limit and good reproducibility. It is suitable for the determination of common plant growth regulator residues in fruits and vegetables.

关 键 词：生长调节剂 超高效液相色谱串联质谱法 同位素内标 水果 蔬菜 污染水平 

分 类 号：R155.54[医药卫生—营养与食品卫生学]