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 0.2 ml/min. The column temperature was set at 40 ℃,and sample size was 5 μl. 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/z 308.2→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). RE-SULTS: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. RS-Ds of intra-day and inter-day were all lower than 15% ;extraction recovery were 88.9% -106.5% ;matrix effect were 94.8%-106.3%. CONCLUSIONS:The method is simple,rapid,sensitive and specific,and it can be used for simultaneous deter-mination of zaleplon,zolpidem and dexzopiclone in human plasma.%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0.9901、0.9968、0.9917），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。
展开▼
