王远　邢丽杰　向晓黎等

摘要

[目的]建立超高效液相色谱串联质谱法（UPLCMS/MS）同时测定葡萄中8种植物生长调节剂残留量的方法。[方法]将供试葡萄样品经乙腈提取，分散固相萃取，采用BEH C18色谱柱分离，以乙腈和水为流动相进行梯度洗脱。采用电喷雾离子化，正负离子分段扫描和多反应监测模式（MRM）检测，外标法定量。[结果]试验得出，缩节胺、矮壮素、赤霉素在2.5 ～500 ng/ml，6苄氨基嘌呤、对氯苯氧乙酸、氯吡脲、多效唑、2，4二氯苯氧乙酸在1～200 ng/ml范围内线性关系良好，相关系数均大于0.990。8种植物生长调节剂的方法检出限为0.2～0.5 μg/kg，方法定量限为0.5～1.5 μg/kg，样品添加回收试验的平均回收率为73.5%～102.2%，相对标准偏差为2.9%～9.7%（n=7）。[结论]该方法简单、灵敏度高、分析时间短，适用于葡萄中8植物生长调节剂的测定。

关键词 超高效液相色谱-串联质谱；植物生长调节剂；残留；葡萄

中图分类号 S481+.8；O657.63 文献标识码

A 文章编号 0517-6611（2015）15-247-05

Determination of 8 Plant Growth Regulator Residues in Grape by UPLCMS/MS

WANG Yuan，XING Lijie，XIANG Xiaoli et al

（Food Quality Supervision and Testing Center of Ministry of Agriculture，Xinjiang Academy of Agricultural Reclamation Science，Shihezi，Xinjiang 832000）

Abstract [Objective] A method was established for determining 8 plant growth regulator residues in grapes by ultra performance liquid chromatographytandem mass spectrometry（UPLCMS/MS）.[Method] Samples were extracted with acetonitrile，and cleaned up dispersivesolid phase extraction.The target analytes were separated on a BEH C18 column with gradient elution using a mobile phase made up of acetonitrile and water.The samples were detected under positive and negative multiple reactions monitoring（MRM） mode through polarity switching between time segments.[Result] The linearities of mepiquat chloride，chlormequat chloride and gibberellic acid were in the concentration range of 2.5-500 ng/ml， 6benzylaminopurine，4chlorophenoxyaceticacid，forchlorfenuron，paclobutrazol and 2，4dichlorophenoxyacetic were in the concentration range of 1-200 ng/ml，with the correlation coefficients higher than 0.990.The limits of detection（LOD） and the limits of quantitation（LOQ） of the method were 0.2-0.5 μg/kg and 0.5-1.5 μg/kg.The average spiked recovery rates were in the range of 73.5%-102.2%.The relative standard deviation（RSD，n=7） was 2.9%-9.7%.[Conclusion] The method proved to be simple，sensitive，rapid and suitable for the determination of 8 plant growth regulator residues in grapes.

Key words Ultra performance liquid chromatographytandem mass spectrometry（UPLCMS/MS）； Plant growth regulator； Residue； Grape

植物生長调节剂（Plant growth regulator，PGRs）是一种能促进植物生长、提高作物产品质量和品质的一类植物激素[1]。植物生长调节剂可分为植物生长促进剂、延缓剂和抑制剂3大类。目前，生产上广泛使用的类别有生长素类（吲哚3乙酸、吲哚3丁酸、α萘乙酸、2，4二氯苯氧乙酸、对氯苯氧乙酸和对氟苯氧乙酸）、细胞分裂素类（异戊烯腺嘌呤、氯吡脲和6苄氨基嘌呤）和赤霉素类等[2]。近年来，由于植物生长调节剂使用不当引起的食品安全问题逐渐增多，植物生长调节剂在农作物中的残留可通过食物链进入人体，轻者造成腹泻等疾病，重者使人体免疫力下降，骨骼疏松，甚至有致畸、致癌、致突变等严重后果[3]。……