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

引用本文: 逄涛, 林茜, 李勇, 师君丽, 邓小鹏, 孔光辉, 卢秀萍, 晋艳. 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[J]. 色谱, 2018, 36(7): 651-658. doi: 10.3724/SP.J.1123.2018.01050 shu

Citation: PANG Tao, LIN Qian, LI Yong, SHI Junli, DENG Xiaopeng, KONG Guanghui, LU Xiuping, JIN Yan. Determination of maleic hydrazide and its glucosides in tobacco leaves using hydrophilic interaction liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(7): 651-658. doi: 10.3724/SP.J.1123.2018.01050 shu

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

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:

English

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

1.
Yunnan Academy of Tobacco Agricultural Sciences, Yuxi 653100, China;
2.
Yuxi Normal University, Yuxi 653100, China
Received Date: 01 February 2018
Fund Project:
Projects of China National Tobacco Corporation Yunnan Branch(Nos. 2017YN11, 2018530000241007, 2018530000241027).

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:

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

1. [1] Schoene D L, Hoffmann O L. Science, 1949, 109(2841):588
2. [2] Barnes J M, Magee P N, Boyland E, et al. Nature, 1957, 180(4576):62
3. [3] Mannell W A, Grice H C. Can J Biochem Physiol, 1957, 35(12):1233
4. [4] Swietlińska Z, Zuk J. Mutat Res, 1978, 55(1):15
5. [5] Codex Alimentarius Pesticides Database Search.[2018-01-29]. http://www.fao.org/fao-who-codexalimentarius/codex-texts/dbs/pestres/pesticide-detail/en/?p_id=102
6. [6] CORESTA Guide No 1. The Concept and Implementation of CPA Guidance Residue Levels.[2018-01-29]. https://www.coresta.org/sites/default/files/technical_documents/main/Guide-No01-GRLs4th-Issue-July16. pdf
7. [7] YQ50-2014. The Maximun Residue Level of Pesticides in Tobacco Leaves. Enterprise Standard of China National Tobacco Corporation, 2014 YQ50-2014. 烟叶农药最大残留量. 中国烟草总公司企业标准, 2014
8. [8] Frear D S, Swanson H R. J Agric Food Chem, 1978, 26:660
9. [9] Tagawa H, Tobita T, Tomita H, et al. Biosci Biotech Biochem, 1995, 59(9):1753
10. [10] Chen X S, Bian Z Y, Yang F, et al. Chinese Journal of Chromatography, 2013, 31(11):1116 陈晓水, 边照阳, 杨飞, 等. 色谱, 2013, 31(11):1116
11. [11] Si X X, Lu S M, Liu Z H, et al. Chinese Journal of Chromatography, 2016, 34(3):340 司晓喜, 陆舍铭, 刘志华, 等. 色谱, 2016, 34(3):340
12. [12] Si X X, Zhu R Z, Zhang F M, et al. Chinese Journal of Chromatography, 2016, 34(6):608 司晓喜, 朱瑞芝, 张凤梅, 等. 色谱, 2016, 34(6):608
13. [13] Mamani M C, Stadler T, da Silva A A, et al. Talanta, 2012, 89:369
14. [14] Chen X S, Zhu S X, Jiang J L, et al. Journal of Chinese Mass Spectrometry Society, 2017, 38(2):234 陈晓水, 朱书秀, 蒋佳磊, 等. 质谱学报, 2017, 38(2):234
15. [15] Wang L, Fei T, Qi D, et al. Anal Methods, 2015, 7:5103
16. [16] Newsome W H. J Agric Food Chem, 1980, 28(2):270
17. [17] Gong C R, Zhou Y H, Yang H W. Introduction for Three Stages Curing of Flue-Cured Tobacco. Beijing:Science Press, 2006 宫长荣, 周义和, 杨焕文. 烤烟三段式烘烤导论. 北京:科学出版社, 2006
18. [18] Dattilo B S, Gallo S, Lionetti G, et al. Beitriige zur Tabakforschung Int, 1994, 16(2):57
19. [19] Paya P, Anastassiades M, Mack D, et al. Anal Bioanal Chem, 2007, 389(6):1697
20. [20] Mamani M C, Stadler T, da Silva A A, Barbosa L C A, et al. Talanta, 2012, 89:369
21. [21] Towers G H N, Hutchinson A. Nature, 1958, 181:1535
22. [22] Guidance Document on Analytical Quality Control and Method Validation Procedures for Pesticides Residues Analysis in Food and Feed.[2018-01-29]. https://ec.europa.eu/food/sites/food/files/plant/docs/pesticides_mrl_guidelines _wrkdoc_2017-11813.pdf

扫一扫看文章

计量

PDF下载量: 3
文章访问数: 396
HTML全文浏览量: 36

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs