UPLC-MS/MS法测定卡泊芬净血浆浓度

中国临床药理学与治疗学 ›› 2017, Vol. 22 ›› Issue (10): 1133-1137.

UPLC-MS/MS法测定卡泊芬净血浆浓度

邵华，何子剑，胡琳璘，詹莹，胡蓉蓉，何杰

东南大学附属中大医院药学部，南京 210009，江苏

收稿日期:2017-07-19 修回日期:2017-10-18 出版日期:2017-10-26 发布日期:2017-11-13
通讯作者: 何杰，女，硕士，研究方向：药物分析。 Tel：15205190695 E-mail：13011014975@163.com
作者简介:邵华，女，博士，副主任药师，硕导，主要从事抗菌药物研究。 Tel：13851725783 E-mail：gycsh@163.com
基金资助:
江苏省自然科学基金（BK20150645）

Determination of caspofungin in human plasma by UPLC-MS/MS

SHAO Hua, HE Zijian, HU Linlin, ZHAN Ying, HU Rongrong, HE Jie

Department of Pharmacy, Zhongda Hospital of Southeast University, Nanjing 210009, Jiangsu, China

Received:2017-07-19 Revised:2017-10-18 Online:2017-10-26 Published:2017-11-13

摘要/Abstract

摘要：

目的: 建立UPLC-MS/MS法测定血浆中卡泊芬净的浓度。方法: 采用AQ C₁₈色谱柱(100 mm×2.1 mm, 3 μm)，柱温40 ℃，流动相为甲醇和0.2%甲酸5 mmol/L乙酸铵水溶液梯度洗脱，流速0.4 mL/min，电喷雾离子化，正离子扫描模式下，卡泊芬净m/z 547.5→538.5，罗红霉素m/z 838.6→157.9（内标），分析时长6.5 min。结果: 卡泊芬净在0.1~25 μg/mL中呈良好的线性关系（R²=0.999 5）；定量下限为0.1 μg/mL；提取回收率为59.08%；日内及日间RSD<15%、准确度、精密度、稳定性等均符合生物样品测定要求。低、中、高和定量下线浓度点的卡泊芬净提取回收率相一致。结论: 本方法操作简单、快捷、准确、灵敏度高且重现性良好，适用于临床上对卡泊芬净血药浓度的快速监测。

关键词: 卡泊芬净, UPLC-MS/MS法, 治疗药物监测

Abstract:

AIM: To establish a method to determine the concentration of caspofungin in human plasma by UPLC-MS/MS. METHODS: Plasma samples were spiked with roxioxithromycin as the internal standard and precipitated by methanol. The column was Ultimate AQ C₁₈ (100 mm×2.1 mm,3 μm) with the column temperature of 40 ℃. The mobile phase was acetonitrile and aqueous solution (5 mmol/L ammonium acetate, 0.2% formic acid), and the pump flow rate was 0.4 mL/min. The ion transitions were performed under ESI positive MRM model at m/z 547.5→538.2 for caspofungin and m/z 838.6→157.9 for internal standard. The analysis time was 6.5 min. RESULTS: Calibration curves of caspofungin showed good linear regression in the range of 0.1-25 μg/mL (R ²=0.999 5). The lowest quantification limit of caspofungin was 0.1 μg/mL. The extraction recovery was about 59.08%. The intra-day and inter-day relative standard deviation (RSD) were less than 15%. CONCLUSION: The established method is simple, accurate, sensitive and had good reproducibility, which can be used for the blood concentration determination of caspofungin.

Key words: caspofungin, UPLC-MS/MS, therapeutics drug monitoring

中图分类号:

R969

邵华，何子剑，胡琳璘，詹莹，胡蓉蓉，何杰. UPLC-MS/MS法测定卡泊芬净血浆浓度[J]. 中国临床药理学与治疗学, 2017, 22(10): 1133-1137.

SHAO Hua, HE Zijian, HU Linlin, ZHAN Ying, HU Rongrong, HE Jie. Determination of caspofungin in human plasma by UPLC-MS/MS[J]. Chinese Journal of Clinical Pharmacology and Therapeutics, 2017, 22(10): 1133-1137.

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