UPLC-MS/MS法测定卡泊芬净血浆浓度  被引量:3

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

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作  者:邵华[1] 何子剑 胡琳璘 詹莹[1] 胡蓉蓉 何杰[1] SHAO Hua;HE Zijian;HU Linlin;ZHAN Ying;HU Rongrong;HE Jie(Department of Pharmacy, Zhongda Hospital of Southeast University, Nanjing 210009, Jiangsu, China)

机构地区:[1]东南大学附属中大医院药学部,江苏南京210009

出  处:《中国临床药理学与治疗学》2017年第10期1133-1137,共5页Chinese Journal of Clinical Pharmacology and Therapeutics

基  金:江苏省自然科学基金(BK20150645)

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 C_(18)色谱柱(100mm×2.1 mm,3μm),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/z838.6→157.9(内标),分析时长6.5 min。结果:卡泊芬净在0.1~25μg/mL中呈良好的线性关系(R^2=0.9995);定量下限为0.1μg/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。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 ClS ( 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 (R2 = 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.

关 键 词:卡泊芬净 UPLC—MS/MS法 治疗药物监测 

分 类 号:R969[医药卫生—药理学]

 

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