LC-MS/MS法测定人血浆中氨基葡萄糖的浓度

doi:10.3969/j.issn.1006-7795.2013.05.016

首都医科大学学报 ›› 2013, Vol. 34 ›› Issue (5): 715-719.doi: 10.3969/j.issn.1006-7795.2013.05.016

LC-MS/MS法测定人血浆中氨基葡萄糖的浓度

李鹏飞¹, 王淑民², 张茜¹, 安卓玲¹, 刘丽宏¹

1. 首都医科大学附属北京朝阳医院药事部, 北京 100020;
2. 首都医科大学附属北京同仁医院药物临床研究室, 北京 100730

收稿日期:2013-03-04 出版日期:2013-10-21 发布日期:2013-10-22
通讯作者: 刘丽宏 E-mail:hongllh@126.com

Determination of glucosamine in human plasma by LC-MS/MS

LI Pengfei¹, WANG Shumin², ZHANG Xi¹, AN Zhuoling¹, LIU Lihong¹

1. Department of Pharmacy Beijing Chao-yang Hospital, Capital Medical University, Beijing 100020, China;
2. Base for Drug Clinical Trial, Beijing Tongren Hospital, Capital Medical University, Beijing 1000730, China

Received:2013-03-04 Online:2013-10-21 Published:2013-10-22

摘要/Abstract

摘要：

目的建立高效液相色谱-质谱联用法测定人血浆中氨基葡萄糖的浓度。方法选用Agilent TC-C₁₈色谱柱,以乙腈-0.01%氨水为流动相,采用梯度洗脱进行分离,样本先用5%磺基水杨酸沉淀,上清液用二氯甲烷液-液萃取后进样,选用3200QTRAP型质谱仪的多重反应监测扫描方式进行检测。结果氨基葡萄糖线性范围为20.0~2 000.0 ng/mL,定量下限为20.0 ng/mL。准确度与精密度结果显示方法日间、日内变异均小于15%,相对偏差为-0.30%~1.69%,低、中、高3个浓度提取回收率为93.59%~106.27%,稳定性较好。结论该方法快速、灵敏、专属性强、重现性高,可用于人体氨基葡萄糖血药浓度的监测,及其制剂的人体药代动力学研究。

关键词: 高效液相色谱-质谱联用法, 氨基葡萄糖, 药代动力学

Abstract:

Objective To develop a LC-MS/MS method for the determination of glucosamine in human plasma. MethodsGlucosamine was extracted with dichloromethane from the supernatant after protein precipitation with 5% sulfosalicylic acid and separated by gradient elution on an Agilent TC-C₁₈ column using acetonitrile -0.01% ammonia water as mobile phase. Detection was carried out by multiple reaction monitoring (MRM) on a 3200QTRAP LC-MS/MS system. Results The assay was linear over the range 20.0~2 000.0 ng/mL with a lower limit of quantitation of 20.0 ng/mL. The intra-and inter-day precision were less than 15%. The relative deviation was in the range -0.30%~1.69%. The recovery of glucosamine was in the range of 93.59%~106.27%.Conclusion The method is a rapid, sensitive, selective and reliable one for the determination of glucosamine in human plasma. The assay could be applied to a pharmacokinetic study in healthy volunteers.

Key words: LC-MS/MS, glucosamine, pharmacokinetics

中图分类号:

李鹏飞, 王淑民, 张茜, 安卓玲, 刘丽宏. LC-MS/MS法测定人血浆中氨基葡萄糖的浓度[J]. 首都医科大学学报, 2013, 34(5): 715-719.

LI Pengfei, WANG Shumin, ZHANG Xi, AN Zhuoling, LIU Lihong. Determination of glucosamine in human plasma by LC-MS/MS[J]. Journal of Capital Medical University, 2013, 34(5): 715-719.

参考文献

[1] 董振香. 葡立胶囊[J]. 中国新药杂志, 2003, 12(7): 572-572.
[2] Zhu Y, Zou J, Xiao D, et al. Bioequivalence of two formulations of glucosamine sulfate 500 mg capsules in healthy male Chinese volunteers: an open-label, randomized-sequence, single-dose, fasting, two-way crossover study [J]. Clin Ther,2009, 31(7): 1551-1558.
[3] 潘杰, 张全英, 张逸凡,等. LC-MS/MS法测定人血浆中硫酸氨基葡萄糖的浓度及其人体生物等效性[J]. 中国临床药学杂志,2009, 18(6): 341-345.
[4] Zhong S, Zhong D, Chen X. Improved and simpli? ed liquid chromatography/electrospray ionization mass spectrometry method for the analysis of underivatized glucosamine in human plasma [J]. J Chromatogr B Analyt Technol Biomed Life Sci, 2007, 854(1-2): 291-298.
[5] 冷艳霞,孙璐, 邸欣,等. 盐酸氨基葡萄糖片的相对生物利用度及其生物等效性评价[J]. 沈阳药科大学学报, 2006, 23(1): 6-9.
[6] 周燕文,徐爱兰, 兰聪贤. 盐酸氨基葡萄糖颗粒在健康人体的药代动力学和相对生物利用度[J]. 中国临床药理学杂志,2008, 24(6): 509-512.
[7] Zhang L J, Huang T M, Fang X L, et al. Determination of glucosamine sulfate in human plasma by precolumn derivatization using high performance liquid chromatography with? uorescence detection: Its application to a bioequivalence study [J]. J Chromatogra B Analyt Technol Biomed Life Sci, 2006, 842(1): 8-12.
[8] 王珵, 宋敏, 王玉. 衍生化LC-MS/MS法测定人血浆中氨基葡萄糖的浓度及药代动力学研究[J]. 药学进展, 2010, 34 (11): 511-517.
[9] Persiani S, Roda E, Rovati LC, et al. Glucosamine oral bioavailability and plasma pharmacokinetics after increasing doses of crystalline glucosamine sulfate in man [J]. OsteoArthritis Cartilage, 2005, 13(12):1041-1049.
[10] 张建伟, 樊媛洁. 氨基葡萄糖苷类化合物的合成研究[J]. 首都医科大学学报,2012,33(5):653-655.
[11] 王太亮, 裴璐,李佳侬.氨糖美辛肠溶胶囊中盐酸氨基葡萄糖含量的测定[J]. 中国煤炭工业医学杂志,2010,13(3):330-331.

LC-MS/MS法测定人血浆中氨基葡萄糖的浓度

Determination of glucosamine in human plasma by LC-MS/MS

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