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园艺学报 ›› 2016, Vol. 43 ›› Issue (1): 175-182.doi: 10.16420/j.issn.0513-353x.2015-0413

• 新方法 • 上一篇    下一篇

超高效液相色谱—串联质谱法检测水果中6种植物生长调节剂

闫 震,聂继云*,徐国锋,李海飞,李 静,李志霞,毋永龙,匡立学   

  1. 中国农业科学院果树研究所,农业部果品质量安全风险评估实验室(兴城),农业部果品及苗木质量监督检验测试中心(兴城),辽宁兴城 125100
  • 出版日期:2016-01-25 发布日期:2016-01-25
  • 基金资助:

    国家农产品质量安全风险评估计划项目(GJFP2015002,GJFP2016002);中国农业科学院科技创新工程项目(CAAS-ASTIP);
    中央级公益性科研院所基本科研业务费专项(0032014013)

Determination of Six Plant Growth Regulators in Fruits by Ultra Performance Liquid Chromatograph–Tandem Mass Spectrometry

YAN Zhen,NIE Ji-yun*,XU Guo-feng,LI Hai-fei,LI Jing,LI Zhi-xia,WU Yong-long,and KUANG Li-xue   

  1. Quality Inspection and Test Center for Fruit and Nursery Stocks,Ministry of Agriculture;Laboratory of Quality and Safety Risk Assessment for Fruit(Xingcheng),Ministry of Agriculture;Institute of Pomology,Chinese Academy of Agricultural Sciences,Xingcheng,Liaoning 125100,China
  • Online:2016-01-25 Published:2016-01-25

摘要:

以苹果、葡萄、猕猴桃、桃和脐橙为试材,建立了水果中6种常用植物生长调节剂(矮壮素、赤霉素、氯吡脲、多效唑、噻苯隆和2,4-D)的超高效液相色谱—串联质谱检测方法(UPLC–MS/MS)。试样采用改进的QuEChERS方法进行前处理,用1%醋酸乙腈提取,选择ODS + MgSO4进行净化,采用电喷雾离子源(ESI)多反应监测(MRM)模式检测,外标定量法。结果表明,6种植物生长调节剂在1 ~ 100 μg · kg-1质量浓度范围内线性关系良好,相关系数均大于0.999,4个添加水平下(1、20、50和100 μg · kg-1)的加标回收率在60.77% ~ 119.43%之间,相对标准偏差(RSD)在0.18% ~ 32.94%之间。苹果、葡萄、猕猴桃、桃和脐橙中6种植物生长调节的检出限(S/N = 3)依次为0.01 ~ 0.14、0.01 ~ 0.18、0.01 ~ 0.08、0.003 ~ 0.11和0.01 ~ 0.08 μg · kg-1,定量限(S/N = 10)依次为0.02 ~ 0.46、0.03 ~ 0.59、0.04 ~ 0.28、0.01 ~ 0.38和0.03 ~ 0.25 μg · kg-1。

关键词: 果实, 超高效液相色谱&mdash, 串联质谱, 植物生长调节剂

Abstract:

Six plant growth regulators frequently used in five fruits of apple,grape,peach,navel orange and kiwifruit were determined by UPLC–MS/MS including chlormequat chloride,GA3,forchlorfenuron,paclobutrazol,thidiazuron and 2,4-D. A modified QuEChERS method was used in pretreatment:Extracted with acetonitrile containing 1% acetic acid,cleaned up by the mixture of ODS and MgSO4. The detection was performed with electrospray ionization(ESI)using multiple reaction monitoring mode,and quantified by the external standard method. The result indicated that the calibrationcurves of six plant growth regulators were linear in the range of 1–100 μg · kg-1 with correlation coefficients over 0.999. The recoveries at four spiked concentration levels of 1,20,50,100 μg · kg-1 ranged from 60.77% to 119.43% and RSD were between 0.18% and 32.94%. The limits of detection(LOD)and limits of quantitation(LOQ)were 0.01–0.14 μg · kg-1 and 0.02–0.46 μg · kg-1 for apple,0.01–0.18 μg · kg-1 and 0.03–0.59 μg · kg-1 for grape,0.01–0.08 μg · kg-1 and 0.04–0.28 μg · kg-1 for kiwifruit,0.003–0.11 μg · kg-1 and 0.01–0.38 μg · kg-1 for peach,0.01–0.08 μg · kg-1 and 0.03–0.25 μg · kg-1 for navel orange,respectively.

Key words: fruit, UPLC–MS/MS, plant growth regulator

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