色谱

色谱 ›› 2014, Vol. 32 ›› Issue (7): 707-716.DOI: 10.3724/SP.J.1123.2014.03003

• 研究论文 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量

黄何何1,2, 张缙1, 徐敦明1, 周昱1, 罗佳2, 吕美玲3, 陈树宾4, 王连珠1   

  1. 1. 厦门出入境检验检疫局, 福建 厦门 361026;
    2. 福建农林大学, 福建 福州 350002;
    3. 安捷伦科技(中国)有限公司, 北京 100102;
    4. 宁波出入境检验检疫局, 浙江 宁波 315000
  • 收稿日期:2014-03-05 修回日期:2014-04-17 出版日期:2014-07-08 发布日期:2014-06-25
  • 通讯作者: 徐敦明，E-mail：Xudm@xmciq.gov.cn.
  • 基金资助:

    福建省自然科学基金项目（2013J01031）；浙江省公益性技术应用研究计划项目（2012C37074）.

Determination of 21 plant growth regulator residues in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry

HUANG Hehe1,2, ZHANG Jin1, XU Dunming1, ZHOU Yu1, LUO Jia2, LV Meiling3, CHEN Shubin4, WANG Lianzhu1   

  1. 1. Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China;
    2. Fujian Agriculture and Forestry University, Fuzhou 350002, China;
    3. Agilent Technologies (China) Limited, Beijing 100102, China;
    4. Ningbo Entry-Exit Inspection and Quarantine Bureau, Ningbo 315000, China
  • Received:2014-03-05 Revised:2014-04-17 Online:2014-07-08 Published:2014-06-25

PDF

729

被引次数

102

摘要：

建立了高效液相色谱-串联质谱法（HPLC-MS/MS）同时测定水果中21种植物生长调节剂残留量的方法。样品经QuEChERS法进行预处理，选用含1%（v/v）乙酸的乙腈溶液提取，无水硫酸镁和十八烷基硅烷（C18）粉末净化，以C18色谱柱分离待测物，采用鞘流电喷雾离子化，正负离子分段扫描和多反应监测模式（MRM）检测，基质匹配标准溶液外标法定量。矮壮素、助壮素、氯化胆碱、环丙酸酰胺、氯吡脲、噻苯隆、抗倒胺、多效唑、烯效唑和抑芽唑在0.10~500 μg/L，丁酰肼和6-苄氨基嘌呤在1.0~500 μg/L，2，3，5-三碘苯甲酸、2，4-D、调果酸、对氯苯氧乙酸（4-CPA）和抗倒酯在2.0~1000 μg/L，赤霉素（GA3）、脱落酸（ABA）、1-萘乙酸（NAA）和吲哚-3-乙酸（IAA）在10~1000 μg/L的范围内线性关系良好，相关系数均大于0.990。21种植物生长调节剂的方法检出限为0.020~6.0 μg/kg，方法定量限为0.10~15.0 μg/kg，样品添加回收试验的平均回收率为73.0%~111.0%，相对标准偏差为3.0%~17.2%（n=6）。该方法快速简便，定量准确，可满足多种水果中21种植物生长调节剂的残留检测要求。

关键词: QuEChERS, 高效液相色谱-串联质谱法, 水果, 植物生长调节剂

Abstract:

A method for the simultaneous detection of 21 plant growth regulators in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed. The samples were initially extracted with acetonitrile containing 1%(v/v) acetic acid, followed by clean-up using the powder of magnesium sulfate and C18. The resulting samples were separated on a C18 column, and detected under positive and negative multiple reactions monitoring (MRM) mode through polarity switching between time segments. The matrix-matched external standard calibration curves were used for quantitative analysis. The linearities of chlormequat chloride, mepiquat chloride, choline chloride, cyclanilide, forchlorfenuron, thidiazuron, inabenfide, paclobutrazol, uniconazole and triapenthenol were in the concentration range of 0.1-500 μg/L, daminozide and 6-benzylaminopurine in the concentration range of 1.0-500 μg/L, 2,3,5-triiodobenzoic acid, 2,4-D, cloprop, 4-chlorophenoxyacetic acid (4-CPA) and trinexapac-ethyl in the concentration range of 2.0-1000 μg/L, abscisic acid (ABA), gibberellic acid (GA3), 1-naphthaleneacetic acid (NAA) and indol-3-ylacetic acid (IAA) in the concentration range of 10-1000 μg/L, with the correlation coefficients higher than 0.990. The limits of detection and the limits of quantification of the method were 0.020-6.0 μg/kg and 0.10-15.0 μg/kg, respectively. For all the samples, the average spiked recoveries ranged from 73.0% to 111.0%, and the relative standard deviations (RSDs, n=6) were in the range of 3.0%-17.2%. The method is quick, easy, effective, sensitive and accurate, and can meet the requirements for the determination of the 21 plant growth regulator residues in fruits.

Key words: fruits, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), plant growth regulators, QuEChERS

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