德拉马尼血药浓度测定方法的建立及应用 点击下载
论文标题: 德拉马尼血药浓度测定方法的建立及应用
英文标题:
中文摘要: 目的 建立测定德拉马尼(DLM)血药浓度的方法并应用。方法血浆样品经甲醇沉淀蛋白后,采用超高效液相色谱-串联质谱(LC-MS/MS)法检测。色谱柱为PhenomenexSynergiTMFusion-RP,流动相为甲醇-0.1%甲酸溶液(梯度洗脱),柱温为40℃,流速为0.3mL/min,进样量为1μL;离子源为电喷雾离子源,以多反应监测模式进行正离子扫描,用于定量分析的DLM离子对为m/z535.0→352.0。采用上述LC-MS/MS法测定6例耐多药结核病(MDR-TB)患者体内DLM的血药浓度。结果DLM检测质量浓度的线性范围为0.05~8μg/mL(r=0.9995),定量下限为0.05μg/mL;日内、日间精密度RSD均小于10%,准确度为92.7%~104.9%,平均基质效应为94.3%~107.5%,平均萃取回收率为93.2%~98.1%。6例MDR-TB患者体内DLM的血药浓度为0.61~2.76μg/mL,平均(1.67±0.74)μg/mL。结论所建LC-MS/MS法专属性好,灵敏度、准确度及精密度均高,可用于MDR-TB患者体内DLM血药浓度的检测。
英文摘要: OBJECTIVE To establish and apply a method for the determination of plasma concentration of delamanid (DLM). METHODS After plasma samples were treated with methanol precipitation, LC-MS/MS was adopted to determine the plasma concentration of DLM. The chromatographic column was Phenomenex SynergiTM Fusion-RP with mobile phase of methanol-0.1% formic acid solution (gradient elution). The column temperature was 40 ℃ , the flow rate was 0.3 mL/min, and the sample size was 1 μL. The ion source was electrospray ion source, and positive ion scanning was carried out in multi-reaction monitoring mode. The DLM ion pair used for quantitative analysis was m/z 535.0→352.0. The plasma concentration of DLM in 6 multidrug resistant tuberculosis (MDR-TB) patients were determined by the LC-MS/MS method. RESULTS The linear range of DLM was 0.05-8 μg/mL (r=0.999 5), and the lowest limit of quantitation was 0.05 μg/mL. RSDs of intra-batch and inter-batch precision were all less than 10%. The accuracy ranged 92.7%-104.9%. Average matrix effect was 94.3%-107.5%. Average recoveries were 93.2%-98.1%. The plasma concentration of DLM in 6 MDR-TB patients ranged from 0.61-2.76 μg/mL, with an average of (1.67± 0.74) μg/mL. CONCLUSIONS The established LC-MS/MS analysis method has good specificity, high sensitivity, accuracy and precision, and can be used to determine DLM plasma concentration in MDR-TB patients.
期刊: 2022年第33卷第24期
作者: 丁巧燕,张欢,马丽华,李思思,张宇,周铭
英文作者: DING Qiaoyan,ZHANG Huan,MA Lihua,LI Sisi,ZHANG Yu,ZHOU Ming
关键字: 德拉马尼;血药浓度;耐多药结核病;高效液相色谱-串联质谱法
KEYWORDS: delamanid; plasma concentration; multidrug resistant tuberculosis; LC-MS/MS
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