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UPLC-MS/MS法同时测定患儿血浆中乙胺丁醇及异烟肼的浓度
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| 篇名： | UPLC-MS/MS法同时测定患儿血浆中乙胺丁醇及异烟肼的浓度 |
| TITLE： | |
| 摘要： | 目的：建立同时测定患儿血浆中乙胺丁醇（EMB）及异烟肼（INH）浓度的方法。方法：血浆样品经乙腈沉淀蛋白后，采用超高效液相色谱-串联质谱法（UPLC-MS/MS）测定。以拉米夫定为内标，色谱柱为Waters ACQUITY® UPLC HSS T3，流动相为乙腈-水（含0.05％甲酸及15 mmol/L甲酸铵），梯度洗脱，流速为0.2 ml/min。采用电喷雾离子源，多反应监测方式进行正离子扫描，用于定量分析的离子对分别为m/z 205.2→116.0（EMB）、m/z 138.1→121.1（INH）、m/z 230.2→111.9（内标）。结果：EMB、INH血药浓度分别在10～5 000、50～5 000 ng/ml范围内线性关系良好，定量下限分别为10、50 ng/ml；日内、日间RSD＜15％，相对回收率为98.7％～105.5％。临床检测4例肺结核患儿体内EMB、INH的血药浓度为94.5～99.7、55.1～80.9 ng/ml。结论：该方法分析快速、灵敏度高，适用于患儿EMB、INH血药浓度的监测及药动学研究。 |
| ABSTRACT： | OBJECTIVE： To establish a method for the simultaneous determination of ethambutol （EMB） and isoniazid （INH） in children’s plasma. METHODS： After precipitated with acetonitrile， plasma samples were determined by UPLC-MS/MS method. Using lamivudine as internal standard， Waters ACQUITY® UPLC HSS T3 column was adopted with mobile phase consisted of acetonitrile-water （containing 0.05％ formic acid and 15 mmol/L ammonium formate） in gradient mode at the flow rate of 0.2 ml/min. By ESI， positive ion detection was conducted in MRM mode. The monitoring transition ion-pair was m/z 205.2→116.0 for EMB， m/z 138.1→121.1 for INH and m/z 230.2→111.9 for internal standard. RESULTS： The linear range of EMB and INH was 10-5 000 ng/ml and 50-5 000 ng/ml， respectively； the limits of quantitation were 10 and 50 ng/ml； RSDs of inter-day and intra-day were all lower than 15％ and relative recoveries were 98.7％-105.5％. Plasma concentrations of EMB and INH in 4 children with tuberculosis were 94.5-99.7 and 55.1-80.9 ng/ml. CONCLUSIONS： The method is rapid and sensitive， which suitable for children’s plasma concentration monitoring of EMB and INH and pharmacokinetic study. |
| 期刊： | 2016年第27卷第20期 |
| 作者： | 安静，董占军，张笑丹，刘洪涛 |
| AUTHORS： | AN Jing，DONG Zhanjun，ZHANG Xiaodan，LIU Hongtao |
| 关键字： | 乙胺丁醇；异烟肼；超高效液相色谱-串联质谱法；血药浓度；肺结核；患儿 |
| KEYWORDS： | Ethambutol； Isoniazid； UPLC-MS/MS； Plasma concentration； Pulmonary tuberculosis； Children |
| 阅读数： | 408 次 |
| 本月下载数： | 4 次 |
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