色谱 ›› 2014, Vol. 32 ›› Issue (8): 861-866.DOI: 10.3724/SP.J.1123.2014.03049

• 技术与应用 • 上一篇    下一篇

高效液相色谱-三重四极杆质谱法同时测定羊栖菜5个部位中10种植物激素含量

李艳, 徐继林, 郑立洋, 李敏, 严小军, 骆其君   

  1. 宁波大学海洋学院, 浙江 宁波 315211
  • 收稿日期:2014-03-28 修回日期:2014-05-20 出版日期:2014-08-08 发布日期:2014-08-01
  • 通讯作者: 骆其君,E-mail:luoqijun@nbu.edu.cn
  • 基金资助:

    东海区优势种类扩繁及高效健康养殖技术集成与示范项目(2011BAD13B08).

Simultaneous determination of ten phytohormones in five parts of Sargasum fusiforme (Hary.) Seichell by high performance liquid chromatography-triple quadrupole mass spectrometry

LI Yan, XU Jilin, ZHENG Liyang, LI Min, YAN Xiaojun, LUO Qijun   

  1. School of Marine Sciences, Ningbo University, Ningbo 315211, China
  • Received:2014-03-28 Revised:2014-05-20 Online:2014-08-08 Published:2014-08-01

摘要:

采用高效液相色谱-三重四极杆质谱(HPLC-TQMS),建立了同时分析羊栖菜主分枝、侧分枝、初生叶、次生叶、茎等5个部位中吲哚乙酸、异戊烯腺苷、异戊烯腺嘌呤、反式玉米素核苷、玉米素、独角金内酯、脱落酸、水杨酸、赤霉素、茉莉酸等10种植物激素含量的方法。羊栖菜样品经冷冻干燥后,用甲醇/水/甲酸(15:4:1,v/v/v)(含0.5% BHT)超声提取植物激素,在Hypersil Gold C18色谱柱上,以甲醇和水为流动相进行梯度洗脱,采用电喷雾电离,正/负离子扫描选择反应监测模式进行定量分析。结果表明,10种植物激素在线性范围内的相关系数(r)为0.9989~1.0000;检出限为0.0012~4.6512 μg/L;加标回收率在72.24%~91.31%之间,相对标准偏差均不高于6.59%;在羊栖菜5个部位鲜样中10种植物激素的含量范围为未检出至4041.431 ng/g。本方法具有良好的灵敏度、精密度和回收率,可以用于同时分析多种植物激素。

关键词: 高效液相色谱-三重四极杆质谱, 羊栖菜, 植物激素

Abstract:

A method for the simultaneous determination of indole-3-acetic acid, N6-(2-isopentenyl) adenosine, N6-(2-isopentenyl) adenine, trans-zeatin riboside, zeatin, strigolactone, abscisic acid, salicylic acid, gibberellin A3 and jasmonic acid in five different parts of main branch, lateral branch, primary leaf, secondary leaf and stem of Sargasum fusiforme (Hary.) Seichell was established by high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-TQMS). The samples were extracted with methanol/water/formic acid (15:4:1, v/v/v)(containing 0.5% 2,6-di-tert-butyl-4-methylphenol, BHT) after vacuum freeze-drying. The separation was performed on a Hypersil Gold C18 column by using methanol and water as mobile phases with gradient elution. The analytes were detected by tandem mass spectrometry in selected reaction monitoring (SRM) mode. The electrospray ionization (ESI) source was used for the quantitative analysis in the positive mode or negative mode. Under the optimized conditions, the correlation coefficients (r) of the ten phytohormones were from 0.9989 to 1.0000 in the linear ranges. The detection limits of the ten phytohormones were 0.0012-4.6512 μg/L. The average recoveries were 72.24%-91.31% with the relative standard deviations not more than 6.59%. In the five parts of fresh Sargasum fusiforme (Hary.) Seichell samples, the contents of the ten phytohormones were from not detected to 4041.431 ng/g. This method has good sensitivity, precision, recovery, and can be used to simultaneously determine the phytohormones.

Key words: Sargasum fusiforme (Hary.) Seichell, high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-TQMS), phytohormones

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