色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 1016-1020.DOI: 10.3724/SP.J.1123.2013.06003

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法检测瓜果中的4种植物生长调节剂的残留量

牟艳莉1, 郭德华2, 丁卓平1   

  1. 1. 上海海洋大学食品学院, 上海 201306;
    2. 上海出入境检验检疫局, 上海 200135
  • 收稿日期:2013-06-03 修回日期:2013-07-02 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 丁卓平, 郭德华

Determination of four plant growth regulator residues in amphisarcas by high performance liquid chromatography-tandem mass spectrometry

MOU Yanli1, GUO Dehua2, DING Zhuoping1   

  1. 1. College of Food Science & Technology, Shanghai Ocean University, Shanghai 201306, China;
    2. Shanghai Exit-Entry Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2013-06-03 Revised:2013-07-02 Online:2013-10-28 Published:2013-10-08

PDF

302

被引次数

27

摘要：

建立了用于测定瓜果中多效唑、氯吡脲、异戊烯腺嘌呤和6-苄氨基嘌呤等4种植物生长调节剂残留量的高效液相色谱-串联质谱分析方法。样品用乙腈提取,经阳离子交换固相萃取柱净化后,用Agilent XDB-C18色谱柱分离,以5 mmol/L乙酸铵溶液和含0.1%(体积分数)甲酸的乙腈溶液为流动相进行梯度洗脱。质谱采用电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质匹配标准溶液外标法定量。4种植物生长调节剂在各自的范围内线性很好,相关系数均大于0.999。选取了黄瓜和苹果作为代表性基质进行添加回收试验,定量限(信噪比大于10)在0.04~1.35 μg/kg之间,检出限(信噪比大于3)在0.01~0.41 μg/kg之间,在3个添加水平下回收率范围为81.0%~93.3%,相对标准偏差(RSDs)为3.5%~9.5%。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求,适用于瓜果中这4种植物生长调节剂残留量的检测。

关键词: 残留, 高效液相色谱-串联质谱, 固相萃取, 瓜果, 植物生长调节剂

Abstract:

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of the plant growth regulator (PGR) (paclobutrazol, forchlorfenuron, isopentennyladenine and 6-benzylaminopurine) residues in amphisarcas. The sample was extracted with acetonitrile, then cleaned up by MCX solid phase extraction. The HPLC separation was performed on an Agilent XDB-C18 column with 5 mmol/L ammonium acetate solution and acetonitrile containing 0.1% (volume percentage) formic acid as the mobile phases in a gradient elution mode. The PGRs were determined by MS/MS in positive electrospray ionization mode, and quantified by matrix-matched external standard method. The calibration curves showed good linearity in each range with correlation coefficients greater than 0.999. The limits of quantification (LOQs, S/N>10) were 0.04-1.35 μg/kg and the limits of detection (LODs, S/N>3) were 0.01-0.41 μg/kg for the four PGRs spiked in cucumber and apple. The recoveries of the four PGRs spiked at three levels ranged from 81.0% to 93.3%, with the relative standard deviations (RSDs) of 3.5%-9.5%. The sensitivity, accuracy and precision of the method meet the technical standards of the pesticide determination. Therefore the method can be applied to the determination of the four PGRs in amphisarcas.

Key words: amphisarcas, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), plant growth regulator (PGR), residue, solid phase extraction (SPE)

中图分类号: