摘要
目的以地西泮、阿普唑仑、三唑仑、艾司唑仑作为测定药物,建立固相萃取仪(SPE)提取和超高效液相色谱仪(UPLC)测定血液中苯二氮卓类药物的方法。方法固相萃取以HLB为萃取柱,甲醇为洗脱液;液相色谱法以甲醇∶0. 1%三乙胺-醋酸(p H=4. 50) 60∶40为流动相,流速1 m L/min,二极管阵列检测器(DAD),检测波长230 nm。结果采用内标-标准曲线法,地西泮、艾司唑仑、阿普唑仑、三唑仑在1~200μg/m L内线性关系良好,相关系数(r)均大于0. 997;灵敏度高,液相最小检出限在0. 15~0. 47μg/m L之间;回收率良好,液相色谱法回收率为78%~105%;精密度良好,相对标准偏差RSD均小于5%。结论固相萃取仪结合HLB柱提取血液中苯二氮卓类药物,操作简便快速,回收率高。UPLC-DAD方法有更好的回收率和重现性,对血液中苯二氮卓类药物的检测更为适用。
Objective To establish a model where four kinds of benzodiazepine in the blood,including diazepam,alprazolam,estazolam and triazolam,are extracted by solid phase extraction( SPE) and determined by ultra-performance liquid chromatography( UPLC). Methods HLB was used as column extractor,and methanol as extraction liquid for solid phase extraction. The mobile phase of UPLC was methanol ∶ 0. 1% triethylamine-acetic acid( p H = 4. 50) 60 ∶ 40 with a flow rate of 1 mL/min. Diode array detector( DAD) was used and the determination wavelength was 230 nm. Results The data was processed with the standard curves of internal standard. The calibration curves showed a linear determination range of 1 ~ 200 μg/m L,and a correlation coefficient of more than 0. 997. The method boasted a high sensitivity with the minimum detection limit of UPLC of 0. 15 ~ 0. 47 μg/m L. The rate of recovery of liquid chromatograph turned to be high which was 78%~ 105%. The precision was found to be good with a relative standard deviation( RSD) of less than 5%. Conclusion SPE with HLB column is handy and rapid to extract benzodiazepine in the blood with a high recovery rate. UPLC-DAD features higher recovery rate and better reproducibility,which is more suitable for the determination of benzodiazepine in the blood.
作者
张彪
敖沛尧
靳浩然
张岚
Zhang Biao;Ao Peiyao;Jin Haoran;Zhang Lan(Forensic Center of Public Security of Jinzhou,Jinzhou 121000 China)
出处
《锦州医科大学学报》
CAS
2019年第5期15-17,I0004,I0005,共5页
Journal of Jinzhou Medical University
