色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1012-1016.DOI: 10.3724/SP.J.1123.2012.08022

• 专栏 • 上一篇    下一篇

液相色谱-四极杆飞行时间质谱法快速测定草莓中6种植物生长调节剂的残留量

刘靖靖*, 宫萍, 张晓梅, 王建华, 王境堂   

  1. 山东出入境检验检疫局, 山东 青岛 266002
  • 收稿日期:2012-08-15 修回日期:2012-09-07 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 刘靖靖,工程师,主要从事食品中有害物质及代谢物的检测. E-mail: jing_liu2008@yahoo.cn.
  • 基金资助:

    山东检验检疫局科研计划支持课题(SK201126).

Determination of six plant growth regulator residues in strawberry by liquid chromatography-quadrupoletime of flight mass spectrometry

LIU Jingjing*, GONG Ping, ZHANG Xiaomei, WANG Jianhua, WANG Jingtang   

  1. Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266002, China
  • Received:2012-08-15 Revised:2012-09-07 Online:2012-10-28 Published:2012-10-17

PDF

431

被引次数

34

摘要： 建立了高效液相色谱-四极杆飞行时间串联质谱(HPLC-Q TOF MS)快速检测草莓中2,4-滴、对氯苯氧乙酸、3-吲哚丁酸、氯吡脲、脱落酸、玉米素6种植物生长调节剂的分析方法。样品采用QuEChERS方法(Quick, Easy, Cheap, Effective, Rugged and Safe method)进行前处理(乙腈提取,C18吸附剂净化),采用Eclipse XDB-C8色谱柱(150 mm×4.6 mm, 5 μm),以乙腈-5 mmol/L乙酸铵-0.1%(v/v)甲酸水溶液为流动相,梯度洗脱,Q TOF MS电喷雾负离子模式分析检测。在全扫描采集模式下,以准分子离子峰的峰面积定量,以化合物的精确质量数定性。在Target MS/MS采集模式下,通过碎片离子的精确质量数进一步确证化合物。各化合物在0.005～1.0 mg/L范围内均呈现良好的线性关系,相关系数均大于0.99。6种化合物的检出限为1～5 μg/kg,添加回收率为87%～107%,相对标准偏差(RSD)均小于10%(n=6)。本方法简便快捷,选择性好,灵敏度高,可满足国内外现行法规的限量要求。

关键词: 草莓, 液相色谱-四极杆飞行时间质谱, 植物生长调节剂

Abstract: A novel method was established for the determination of six plant growth regulators (PGRs), 2,4-dichlorophenoxy acetic (2,4-D), 4-chlorophenoxy-acetic acid (CAP), 4-(3-indolyl)-butyric acid (BAA), forchlorfenuron (CPPU), abscisic acid (ABA) and trans-zeatin (ZT) in strawberry using liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q TOF MS). The Quick, Easy, Cheap, Effective, Rugged and Safe method (QuEChERS) has been validated for the extraction. In this QuEChERS method, the sample was extracted by acetonitrile and cleaned up with C18 adsorbent. The extract was measured directly by LC-Q TOF MS with electrospray ionization in negative mode. The compounds were separated on an Eclipse XDB-C8 column (150 mm×4.6 mm, 5 μm) with acetonitrile-5 mmol/L ammonium acetate-0.1% formic acid as mobile phase under gradient elution. The confirmatory analysis was carried out by determining the accurate masses of all compounds and fragment ions upon Target MS/MS. The limits of detection (LODs) were between 1 μg/kg and 5 μg/kg. The linear range was 0.005~1.0 mg/L for each analyte. The recoveries ranged from 87% to 107% with the relative standard deviations (RSDs) less than 10% (n=6). The method was proved to be simple and accurate.

Key words: plant growth regulators, strawberry, liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q TOF MS)

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