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同位素稀释-超高效液相色谱-串联质谱法测定人血浆中氟康唑的浓度
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| 篇名： | 同位素稀释-超高效液相色谱-串联质谱法测定人血浆中氟康唑的浓度 |
| TITLE： | |
| 摘要： | 目的：建立测定人血浆中氟康唑浓度的方法。方法：血浆样品经乙腈沉淀蛋白后，以同位素氟康唑-d4为内标，采用超高效液相色谱-串联质谱法测定。色谱柱为ACQUITY UPLC BEH C18，流动相为0.1％甲酸溶液-乙腈（梯度洗脱），流速为0.3 mL/min，柱温为40 ℃，进样量为3 μL；采用电喷雾离子源，以多反应监测模式进行正离子扫描，用于定量分析的离子对分别为m/z 307.1→220.0（氟康唑）和m/z 311.1→223.0（内标）。结果：氟康唑血药浓度检测的线性范围为10～5 000 ng/mL（r＝0.998 1），定量下限为10 ng/mL；日内、日间RSD均低于8％，准确度为95.8％～106.7％；提取回收率为97.3％～107.3％（RSD＜5.0％，n＝6），基质效应、稀释效应及残留效应均不影响待测物的定量分析。结论：该方法简便、快速、专属性强、准确度高，可用于氟康唑治疗药物监测及药动学研究。 |
| ABSTRACT： | OBJECTIVE： To establish a method for determination of fluconazole concentration in human plasma. METHODS： UPLC-MS/MS method was adopted to determine plasma after precipitated with acetonitrile. Using isotope fluconazole-d4 as internal standard， the determination was performed on ACQUITY UPLC BEH C18 column with mobile phase consisted of 0.1％ formic acid-acetonitrile （gradient elution） at the flow rate of 0.3 mL/min. The column temperature was 40 ℃， and the sample size was 3 μL. ESI was used for positive ion scanning by multiple reaction monitoring mode. The ion pairs for quantitative analysis were m/z 307.1→220.0 （fluconazole） and m/z 311.1→223.0 （internal standard）. RESULTS： The linear range of fluconazole was 10-5 000 ng/mL （r＝0.998 1）. The limits of quantitation was 10 ng/mL. RSDs of intra-day and inter-day were less than 8％； accuracy ranged 95.8％-106.7％. The extraction recovery ranged 97.3％-107.3％ （RSD＜5.0％， n＝6）， and matrix effect， dilution effect and residual effect didn’t influence quantitative analysis of the substance to be measured. CONCLUSIONS： The method is simple， rapid， specific and accurate， which can be used for therapeutic drug monitoring and pharmacokinetic study of fluconazole. |
| 期刊： | 2019年第30卷第2期 |
| 作者： | 杨浩天，吴茵，宋浩静，邱志宏，董占军 |
| AUTHORS： | YANG Haotian，WU Yin，SONG Haojing，QIU Zhihong，DONG Zhanjun |
| 关键字： | 氟康唑；同位素内标；超高效液相色谱-串联质谱法；血药浓度；治疗药物监测 |
| KEYWORDS： | Fluconazole； Isotope internal standard； UPLC-MS/MS； Plasma concentration； Therapeutic drug monitoring |
| 阅读数： | 290 次 |
| 本月下载数： | 6 次 |
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