超高效液相色谱-串联质谱法同时测定果蔬中6种植物生长调节剂

Detection of six plant growth regulators in vegetables and fruits by using ultra high performance liquid chromatography mass/mass spectrometry method

目的建立果蔬中6-苄基腺嘌呤、赤霉素、氯吡脲、噻苯隆、4-氯苯氧乙酸和2,4-二氯苯氧乙酸的超高效液相色谱-串联质谱测定方法(UPLC-MS/MS)。方法样品经1%(V/V)乙酸-乙腈提取后加入脱水试剂脱水,取上清液加入基质分散固相萃取试剂净化,过膜后以乙腈与0.1%甲酸-5 mmoL/L甲酸铵溶液梯度洗脱,经Waters Acquity HSS T3(2.1 mm×100 mm,1.8μm)色谱柱分离,最后在质谱多反应监测(MRM)模式下分析,6种植物生长调节剂均用负离子(ESI-)模式检测。结果 6种植物生长调节剂在1～200μg/L范围内,线性关系良好(r≥0.9913),各组分检出限为0.242～0.508μg/kg,回收率为69.1%～105.0%,RSD为1.04%～5.06%。结论 UPLC-MS/MS法简便、快速、准确,可用于食品中果蔬中6种植物生长调节剂的检测。

Objective To develop a method for detecting 6 benzyl adenine,gibberellin,forchlorfenuron,thidiazuron,4 chlorobenzoxy acetic acid and 2,4 dichlorophenoxyacetic acid in vegetables and fruits by using ultra performance liquid chromatography mass/mass spectrometry method(UPLC-MS/MS).Methods The samples were extracted by 1%(V/V)acetonitrile-acetic acid,purified by matrix solid phase dispersion method after being dehydrated with dehydration reagents,and eluted by acetonitrile and 0.1%formic acid and 5 mmoL/L ammonium formate solution after being filtered by microporous filter membrane.The samples were separated on a ACQUITY HSS T3(1.8μm,2.1 mm×100 mm)column,and then analyzed in the multiple reactions monitoring(MRM)mode.The six kinds of plant growth regulators were all detected with negative mode.Results The six kinds of plant growth regulators showed a good linearity in the rang of 1-200μg/L(r≥0.9913).The detection limits were 0.242-0.508μg/kg,the recovery rates were 69.1%-105.0%and values of RSD were 1.04%-5.06%.Conclusion The UPLC-MS/MS method was simple,quick and accurate,and suitable for the detection of six plant growth regulators in vegetables and fruits.