液相色谱-质谱联用方法测定大鼠血浆、尿液及结肠组织中美沙拉嗪及其代谢产物N-乙酰-5-ASA的浓度

饶志,秦红岩,邵云云,黄静,武新安*

中国药学杂志 ›› 2014, Vol. 49 ›› Issue (14) : 1252-1257.

PDF(1678 KB)
PDF(1678 KB)
中国药学杂志 ›› 2014, Vol. 49 ›› Issue (14) : 1252-1257. DOI: 10.11669/cpj.2014.14.019
论著

液相色谱-质谱联用方法测定大鼠血浆、尿液及结肠组织中美沙拉嗪及其代谢产物N-乙酰-5-ASA的浓度

  • 饶志1,秦红岩1,邵云云12,黄静12,武新安1*
作者信息 +

Development of LC-MS/MS Method for Determination of Mesalazine and N-Ac-5-ASA in Rat Plasma, Urine and Colon

  • RAO Zhi1, QIN Hong-yan1, SHAO Yun-yun1,2, HUANG Jing1,2, WU Xin-an1*
Author information +
文章历史 +

摘要

目的 建立应用LC-MS/MS进行大鼠血浆、尿液、结肠中美沙拉嗪及其体内代谢物N-乙酰-5-ASA浓度的测定方法,并将其应用于美沙拉嗪及N-乙酰-5-ASA在大鼠体内过程的研究。方法 血浆、尿液及结肠样品均用甲醇沉淀蛋白进行提取,以ESI电离源在负离子模式下检测,用Agilent HC-C18色谱柱,甲醇-醋酸水溶液为流动相梯度洗脱,流速为1.0 mL·min-1。结果 美沙拉嗪及N-乙酰-5-ASA在大鼠血浆、尿液及结肠中的线性范围及定量限均符合测定要求,日内、日间精密度及基质效应均 < 15%。结论 本方法快速、灵敏、专属性强且重现性好,可用于大鼠血浆、尿液、结肠中美沙拉嗪及N-乙酰-5-ASA测定。

Abstract

OBJECTIVE To develop an LC-MS/MS method for determination of mesalazine and its metabolite, N-Ac-5-ASA, in rat plasma, urine and colon for the pharmacokinetic study of mesalazine and N-Ac-5-ASA in rats. METHODS The plasma, urine and colon samples were treated with methanol to precipitate protein. An Agilent HC-C18 column was used as the analytical column, with methanol and acetic acid aqueous solution as mobile phase eluted by a gradient program at a flow rate of 1.0 mL穖in-1. The detection was accomplished with ESI source operated in negative ionization mode. RESULTS The linearity and LLOQs of mesalazine and N-Ac-5-ASA in rat plasma, urine and colon both met the requirements, and the inter- and intra-day RSDs and matrix effect were less than 15%. CONCLUSION This assay is a rapid, sensitive, selective and reliable method for determination of mesalazine and N-Ac-5-ASA in rat plasma, urine and colon.

关键词

高效液相色谱-质谱联用 / 美沙拉嗪 / N-乙酰-5-ASA

Key words

LC-MS/MS / mesalazine / N-Ac-5-ASA

引用本文

导出引用
饶志,秦红岩,邵云云,黄静,武新安*. 液相色谱-质谱联用方法测定大鼠血浆、尿液及结肠组织中美沙拉嗪及其代谢产物N-乙酰-5-ASA的浓度[J]. 中国药学杂志, 2014, 49(14): 1252-1257 https://doi.org/10.11669/cpj.2014.14.019
RAO Zhi, QIN Hong-yan, SHAO Yun-yun,, HUANG Jing,, WU Xin-an* . Development of LC-MS/MS Method for Determination of Mesalazine and N-Ac-5-ASA in Rat Plasma, Urine and Colon[J]. Chinese Pharmaceutical Journal, 2014, 49(14): 1252-1257 https://doi.org/10.11669/cpj.2014.14.019
中图分类号: R917   

参考文献

DOROFEYEV A E, KIRIYAN E A, VASILENKO I V, et al. Clinical, endoscopical and morphological efficacy of mesalazine in patients with irritable bowel syndrome . Clin Exp Gastroenterol, 2011, 4: 141-153. PASTORINI E, LOCATELLI M, SIMONI P, et al. Development and validation of a HPLC-ESI-MS/MS method for the determination of 5-aminosalicylic acid and its major metabolite N-acetyl-5-aminosalicylic acid in human plasma . J Chromatogr B, 2008, 872 (1-2): 99-106. NOBILIS M, VYBIRALOVA Z, SLADKOVA K, et al. High-performance liquid-chromatographic determination of 5-aminosalicylic acid and its metabolites in blood plasma . J Chromatogr A, 2006, 1119 (1-2): 299-308. GANDIA P, IDIER I, HOUIN G. Is once-daily mesalazine equivalent to the currently used twice-daily regimen A study performed in 30 healthy volunteers . J Clin Pharmacol, 2007, 47 (3): 334-342. PALUMBO G, BACCHI S, PRIMAVERA L, et al. A validated HPLC method with electrochemical detection for simultaneous assay of 5-aminosalicylic acid and its metabolite in human plasma . Biomed Chromatogr, 2005, 19 (5): 350-354.
PDF(1678 KB)

38

Accesses

0

Citation

Detail

段落导航
相关文章

/