摘要
目的 采用固相萃取-超高效液相色谱质谱联用技术（SPE-UPLC-MS/MS）同时测定人血浆中的劳拉西泮、艾司唑仑、咪达唑仑、氯硝西泮、扎来普隆、地西泮、奥沙西泮、唑吡坦和三唑仑等9种镇静催眠药。方法 采用Waters Acquity UPLC HSS T3色谱柱（100 mm×2.1 mm,1.8μm）,流动相为乙腈-0.1%氨水溶液,梯度洗脱,流速0.2 mL·min^（-1）,柱温40℃。离子化方式为电喷雾,多反应离子监测,正离子模式。结果 9种被分析物的线性范围除氯硝西泮为0.1~20.0 ng·mL^（-1）外,其余均为0.05~20.00 ng·mL^（-1）,r为0.9967~0.9996。除咪达唑仑在低质控点的日内RSD=15.9%外,其他被分析物的日内、日间RSD均小于12.7%,提取回收率大于52%,基质效应为90.0%~117.0%。结论 所用方法专属性强、快速灵敏,可用于人血浆中9种镇静催眠药的检测。
OBJECTIVE To establish a UPLC - MS/MS method for the simultaneous determination of larazepam, estrazolam, midazo- lam,clonazepam,zaleplone,diazepam,oxazepam, zolpidam and triazolam by solid phase extraction （SPE）. METHODS The mobile phase was consisted of acetonitrile - water（containing 0.1% ammonium） at a flow rate of 0.2 mL min-1 in gradient elution mode. Chromatographic separation was performed with a Waters Acquity UPLC HSS T3 （ 100 mm × 2. 1 mm, 1.8 μm） column and the column temperature was 40 ℃. The ionization was electrospray ionization （ESI） with multiple reaction monitoring （MRM） in positive mode. RESULTS The calibration curves of clonazepam was linear in the range of 0.1 - 20 ng. mL-1 and 0.05 - 20 ng. mL-1 for other sedativehypnotics with correlation coefficients of 0. 9967 - 0. 9996. The intra - and inter - day RSD was no more than 12.7, except that of midazolam was 15.9% near LLOQ. The extraction recoveries were over 52% ,and the matrix effects were in the range of 90.0% - 117.0%. CONCLUSION The method is sensitive and accuracy, and can be applied for the determination of nine kinds of sedativehypnotics in human plasma.
出处
《华西药学杂志》
CAS
CSCD
2018年第1期72-76,共5页
West China Journal of Pharmaceutical Sciences
基金
河北省科技支撑计划项目(编号:14273002D)
