色谱

色谱 ›› 2018, Vol. 36 ›› Issue (7): 651-658.DOI: 10.3724/SP.J.1123.2018.01050

• 研究论文 • 上一篇    下一篇

亲水作用液相色谱-串联质谱测定烟叶中马来酰肼及其糖苷

逄涛1, 林茜2, 李勇1, 师君丽1, 邓小鹏1, 孔光辉1, 卢秀萍1, 晋艳1   

  1. 1. 云南省烟草农业科学研究院, 云南 玉溪 653100;
    2. 玉溪师范学院, 云南 玉溪 653100
  • 收稿日期:2018-02-01 出版日期:2018-07-08 发布日期:2014-06-03
  • 通讯作者: 李勇,Tel:0877,2075095,E-mail:liyong189108@163.com
  • 基金资助:

    中国烟草总公司云南省公司项目（2017YN11，2018530000241007，2018530000241027）.

Determination of maleic hydrazide and its glucosides in tobacco leaves using hydrophilic interaction liquid chromatography-tandem mass spectrometry

PANG Tao1, LIN Qian2, LI Yong1, SHI Junli1, DENG Xiaopeng1, KONG Guanghui1, LU Xiuping1, JIN Yan1   

  1. 1. Yunnan Academy of Tobacco Agricultural Sciences, Yuxi 653100, China;
    2. Yuxi Normal University, Yuxi 653100, China
  • Received:2018-02-01 Online:2018-07-08 Published:2014-06-03
  • Supported by:

    Projects of China National Tobacco Corporation Yunnan Branch(Nos. 2017YN11, 2018530000241007, 2018530000241027).

PDF

65

摘要：

建立了一种基于亲水作用液相色谱-串联质谱的烟叶中马来酰肼及其糖苷的定量分析方法。方法采用乙腈-甲基叔丁基醚-水（7：10：13，体积比）超声波辅助提取烟叶中的马来酰肼及其糖苷，提取液经离心分相和溶剂置换后进行亲水作用液相色谱-串联质谱分析。马来酰肼及马来酰肼-O-β-D-葡萄糖苷的基质添加标准曲线的线性范围为5~150 mg/kg，相关系数（r2）为0.9971及0.9972，检出限分别为0.5 mg/kg和0.3 mg/kg，定量限分别为1.0 mg/kg和0.8 mg/kg。马来酰肼及马来酰肼-O-β-D-葡萄糖苷在10、40、80 mg/kg 3个加标水平下的回收率为83.1%~112.3%，在40 mg/kg加标水平下的日内重复性分别为2.7%和3.8%，日间重复性分别为8.3%和7.1%。应用该方法分析喷洒马来酰肼28天后烟叶中马来酰肼的分布情况，发现马来酰肼含量减少了80.8%，其中仅有7.6%转化成了马来酰肼糖苷，其他马来酰肼的去向有待进一步研究。

关键词: 串联质谱, 马来酰肼, 亲水作用液相色谱, 糖苷, 烟叶

Abstract:

A hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method was established for the simultaneous determination of maleic hydrazide (MH) and its two glucosides in tobacco leaves. Ultrasonic assisted extraction of MH and its glucosides was performed using acetonitrile-methyl tert-butyl ether-water (7:10:13, volume ratio). The extraction solution was then centrifuged, and the subnatant was transferred for solvent replacement using acetonitrile. The extract in acetonitrile was then analyzed using HILIC-MS/MS. Method validation was performed, and the linear ranges for MH and MH-O-β -D-glucoside were 5-150 mg/kg with correlation coefficients (r2) greater than 0.9971 for matrix-matched calibration curves. Limits of detection for MH and MH-O-β -D-glucoside were 0.5 mg/kg and 0.3 mg/kg, and limits of quantification were 1.0 mg/kg and 0.8 mg/kg, respectively. The recoveries were in the range of 83.1%-112.3% at three spiked levels (10, 40, 80 mg/kg), with intra-day repeatability of 2.7% and 3.8%, inter-day repeatability of 8.3% and 7.1% at 40 mg/kg. The established method was used for the study of MH metabolism in tobacco leaves. By the 28th day after MH spraying, the content of MH in tobacco leaves had decreased by 80.8%, of which only 7.6% transformed to MH-glucosides. The disposition of the remainder needs to be studied.

Key words: glucoside, hydrophilic interaction liquid chromatography(HILIC), maleic hydrazide, tandem mass spectrometry(MS/MS), tobacco leaves

中图分类号: