色谱

色谱 ›› 2017, Vol. 35 ›› Issue (9): 963-969.DOI: 10.3724/SP.J.1123.2017.06005

• 研究论文 • 上一篇    下一篇

基质分散固相萃取-高效液相色谱-串联质谱法检测红薯中的植物生长调节剂

张婧, 万慧慧, 张华   

  1. 大连理工大学化工与环境生命学部化学分析测试中心, 辽宁 大连 116024
  • 收稿日期:2017-06-01 出版日期:2017-09-08 发布日期:2017-09-15
  • 通讯作者: 万慧慧,E-mail:wanhuihui@dlut.edu.cn;张华,zhanghua@dlut.edu.cn.
  • 基金资助:

    国家自然科学基金项目（21505014）；大连理工大学引进人才科研专题项目（DUT15RC（4）13）.

Determination of the plant growth regulators in batatas by matrix solid-phase dispersive extraction and high performance liquid chromatography with tandem mass spectrometry

ZHANG Jing, WAN Huihui, ZHANG Hua   

  1. Chemical Analysis and Testing Center, Faculty of Chemical, Environmental and Biological Science and Technology, Dalian University of Technology, Dalian 116024, China
  • Received:2017-06-01 Online:2017-09-08 Published:2017-09-15
  • Supported by:

    National Natural Science Foundation of China (No. 21505014); Dalian University of Technology for Talent Introduction (No. DUT15RC(4)13).

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摘要：

建立了基质分散固相萃取-高效液相色谱-串联质谱测定红薯中氯吡脲、6-苄氨基嘌呤、增效胺以及多效唑含量的方法。样品经硅胶分散剂研磨分散、甲醇洗脱提取后，采用Thermo hypersil GOLD C18色谱柱（150 mm×2.1 mm， 5 μm），以甲醇和0.1%（体积分数）甲酸-5 mmol/L甲酸铵为流动相进行梯度洗脱，在电喷雾离子源正离子或负离子模式下以选择反应监测（SRM）模式检测，外标法定量。氯吡脲、6-苄氨基嘌呤、增效胺和多效唑分别在10.8~216.0、10.8~216.0、12.5~250.0和10.2~204.0 ng/g范围内呈良好的线性关系，相关系数（r2）均大于0.96。以信噪比等于10确定4种植物生长调节剂的定量限，氯吡脲、6-苄氨基嘌呤、增效胺和多效唑的定量限分别为0.1、0.3、0.2和0.1 ng/g。4种植物生长调节剂在50、100及200 ng/g加标水平下的回收率为85.3%~116.0%，相对标准偏差为0.6%~22.7%。该方法操作简单、准确，适用于红薯中氯吡脲、6-苄氨基嘌呤、增效胺以及多效唑的定量检测分析。

关键词: 6-苄氨基嘌呤, 多效唑, 高效液相色谱-串联质谱, 红薯, 基质分散固相萃取, 氯吡脲, 增效胺

Abstract:

An analytical method based on matrix solid-phase dispersive (MSPD) extraction and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established for the determination of forchlorfenuron, 6-benzylaminopurine (6-BA), N-(2-ethylhexyl)-5-norbornene-2,3-dicarboximide (MGK 264) and paclobutrazol in batatas. The samples were dispersed with silica by grinding, and then extracted with methanol. The determination was carried out on a Thermo hypersil GOLD C18 column (150 mm×2.1 mm, 5 μm) in gradient elution with mobile phases of methanol and ammonium formate (5 mmol/L, containing 0.1% (v/v) formic acid) and detected with tandem mass spectrometry using selected reaction monitoring (SRM) mode. The quantification was performed using external standard calibration, and the calibration curves were performed in the ranges of 10.8-216.0 ng/g (forchlorfenuron), 10.8-216.0 ng/g (6-BA), 12.5-250.0 ng/g (MGK 264), 10.2-204.0 ng/g (paclobutrazol) with the correlation coefficients larger than 0.96. The limits of quantification (LOQs) were 0.1-0.3 ng/g. The spiked recoveries at the levels of 50, 100 and 200 ng/g of these four plant growth regulators were in the range of 85.3%-116.0%, and the relative standard deviations were 0.6%-22.7%. This method has advantages of simple operation and good accuracy, and can be used for the quantitative determination of forchlorfenuron, 6-BA, MGK 264 and paclobutrazol in batatas.

Key words: N-(2-ethylhexyl)-5-norbornene-2,3-dicarboximide (MGK 264), 6-benzylaminopurine(6-BA), batata, forchlorfenuron, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), matrix solid-phase dispersive (MSPD), paclobutrazol

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