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
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摘要
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(1.8 μm,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 1-200 μg/L(r≥0.9913). The detection limits were 0.242-0.508 μg/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.
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(1.8 μm,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 1-200 μg/L(r≥0.9913). The detection limits were 0.242-0.508 μg/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.
引文
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[4] 林涛,邵金良,刘兴勇,等.QuEChERS -超高效液相色谱-串联质谱法测定蔬菜中41 种农药残留[J].色谱,2015,33(5):235-241.
[2] CONTRERAS HR,BADILLA J,BUSTOS-OBREGON E.Morphofunctional disturbances of human sperm after incubation with organophosphorate pesticides[J].Biocell,1999, 23(2):135-141.
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[4] 林涛,邵金良,刘兴勇,等.QuEChERS -超高效液相色谱-串联质谱法测定蔬菜中41 种农药残留[J].色谱,2015,33(5):235-241.