摘要
目的：建立快速、准确、可同时检测人血浆中唑吡坦、右佐匹克隆和扎来普隆的分析方法。方法：血浆样品经液-液萃取后,以卡马西平为内标,采用超高效液相色谱-串联质谱法检测。色谱柱为Waters ACQUITY UPLC HSS T3,流动相为0.1%氨水-乙腈（梯度洗脱）,流速为0.2 ml/min,柱温为40℃,进样量为5μl。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 308.2→263.1（唑吡坦）、m/z 389.3→245.0（右佐匹克隆）、m/z 306.2→236.1（扎来普隆）、m/z 237.3→151.2（内标）。结果：唑吡坦、右佐匹克隆、扎来普隆血药浓度分别在0.02~20.00、0.50~20.00、0.02~20.00 ng/ml范围内线性关系良好（r分别为0.990 1、0.996 8、0.991 7）,定量下限分别0.02、0.50、0.02 ng/ml,检测限分别为0.01、0.20、0.01 ng/ml;日内、日间RSD〈15%,提取回收率为88.9%~106.5%,基质效应为94.8%~106.3%。结论：该方法简便、快速、灵敏度高、专属性好,可用于人血浆中唑吡坦、右佐匹克隆和扎来普隆的同时检测。
OBJECTIVE：To develop a method for rapid,accurate and simultaneous determination of dexzopiclone,zolpidam and zaleplon in human plasma. METHODS：After the plasma sample was processed by liquid-liquid extraction,UPLC-MS/MS was established to detect plasma sample with carbamazepine as internal standard. The separation was performed on a Waters ACQUITY UPLC HSS T3 column with mobile phase composed of 0.1% ammonium solution-acetonitrile（gradient elution）at flow rate of 0.2ml/min. The column temperature was set at 40 ℃,and sample size was 5 μ l. The detection was performed by multiple reaction monitoring（MRM）via electrospray ionization（ESI）source in positive mode. The mass transition ion-pairs were as follows：m/z308.2→263.1（zolpidem）,m/z 389.3→245.0（dexzopiclone）,m/z 306.2→236.1（zaleplon）,m/z 237.3→151.2（internal standard）. RESULTS：The linear range of zolpidem,dexzopiclone and zaleplon were 0.02-20.00,0.50-20.00,0.02-20.00 ng/ml,respectively（r=0.990 1,0.996 8,0.991 7）. LLOQ of them were 0.02,0.50,0.02 ng/ml,and detection limit were 0.01,0.20,0.01 ng/ml. RSDs of intra-day and inter-day were all lower than 15%; extraction recovery were 88.9%-106.5%; matrix effect were94.8%-106.3%. CONCLUSIONS：The method is simple,rapid,sensitive and specific,and it can be used for simultaneous determination of zaleplon,zolpidem and dexzopiclone in human plasma.
出处
《中国药房》
CAS
北大核心
2016年第23期3194-3197,共4页
China Pharmacy
基金
河北省科技计划项目(No.14273002D)
