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德拉马尼血药浓度测定方法的建立及应用
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| 篇名： | 德拉马尼血药浓度测定方法的建立及应用 |
| TITLE： | Establishment and application of a method for the determination of plasma concentration of delamanid |
| 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。 |
| ABSTRACT： | 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 |
| AUTHORS： | 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 |
| 阅读数： | 187 次 |
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