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LC-MS/MS法测定人血浆中卡马西平的浓度及其在室间质评中的应用
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| 篇名： | LC-MS/MS法测定人血浆中卡马西平的浓度及其在室间质评中的应用 |
| TITLE： | |
| 摘要： | 目的：建立并验证测定人血浆中卡马西平（CBZ）浓度的方法，并应用于CBZ的室间质评。方法：血浆样品经乙腈沉淀后，采用液相色谱-串联质谱（LC-MS/MS）法测定。内标为氯雷他定，色谱柱为Kromasil C18，流动相为水（含0.1％甲酸）-乙腈，梯度洗脱，流速为0.6 ml/min，柱温为40 ℃；采用电喷雾离子源，以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 237.1→194.0（CBZ）、m/z 383.1→267.0（内标）。结果：CBZ血药浓度在5～1 000 ng/ml范围内线性关系良好（r＞0.998），定量下限为5 ng/ml；日内、日间RSD为1.00％～6.42％，相对偏差为－6.93％～0.32％；5个室间质评样品的检测结果分别为679.0、475.0、104.0、29.2、26.2 ng/ml，评价结果通过率为100％。结论：该方法灵敏、准确、专属性强，可用于CBZ血药浓度测定及其室间质评。 |
| ABSTRACT： | OBJECTIVE： To establish and validate the method for the determination of carbamazepine （CBZ） in human plasma， and to apply the method for external quality assessment. METHODS： After precipitated with acetonitrile， the plasma sample was determined by LC-MS/MS. Using loratadine as internal standard， the determination was performed on Kromasil C18 column with mobile phase consisted of water （containing 0.1％ formic acid）-acetonitrile （gradient elution） at flow rate of 0.6 ml/min and column temperature of 40 ℃. The ion transitions under MRM mode by ESI+ ionization were performed at m/z 237.1→194.0 and m/z 383.1→267.0 for CBZ and internal standard， respectively. RESULTS： The linear range of CBZ were 5-1 000 ng/ml （r＞0.998）. The limit of quantitation was 5 ng/ml. RSDs of inter-day and intra-day were 1.00％-6.42％； relative deviation were －6.93％-0.32％. The external quality assessment of 5 samples were 679.0， 475.0， 104.0， 29.2 and 26.2 ng/ml， respectively. The pass rate of assessment result was 100％. CONCLUSIONS： The method is sensitive， accurate and specific. The method is applicable for the plasma concentration determination and external quality assessment of CBZ. |
| 期刊： | 2016年第27卷第8期 |
| 作者： | 梅升辉，杨莉，冯卫星，赵志刚，朱乐亭 |
| AUTHORS： | MEI Shenghui，YANG Li，FENG Weixing，ZHAO Zhigang，ZHU Leting |
| 关键字： | 液相色谱-串联质谱法；卡马西平；血药浓度；室间质评 |
| KEYWORDS： | LC-MS/MS； Carbamazepine； Plasma concentration； External quality assessment |
| 阅读数： | 624 次 |
| 本月下载数： | 12 次 |
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