固相萃取HPLC/MS法测定血中氯硝安定

Determination of Clonazepam in Blood Sample by SPE-HPLC-MS

目的建立测定人血中氯硝安定的HPLC/MS定性、定量方法。方法在血液中添加氯硝安定,采用固相萃取、HPLC法分离、LC/MS法定性、定量。结果标准氯硝安定LC/MS法的工作曲线在0.5-500ng时为Y=0.655×10^3X＋2.15×10^3,相关系数r=0.9981,最小检出限为0.5ng/m l。结论采用pH8.0的磷酸盐缓冲液进行稀释、C18柱固相萃取氯硝安定回收率较高,优化后固定的LC/MS检测方法简便、快速、准确,适合办案需要。

Objective For the purpose of analysis of Clonazepam in blood, a reversed-phase high performance liquid chromatography-mass spectrum （HPLC/MS） method was developed. Methods Standard Clonazepam was added to the blank blood when the samples were pretreated. The pretreatment methods of samples, the linear range, the precision, the recoveries, quantitative and qualitative method by HPLC/ MS were investigated Results The Clonazepam linear range were 0.5 - 500.0 ng/ml,γ =0.9981. The detective limits were 0.5ng/ml. Conclusion Higher recovery was obtained by C18 extraction with the dilution of phosphate buffer （pH8.0）. The quantitative and qualitative method for clonazepam by HPLC/MS is simple, rapid and accurate. It is suitable for the concentration monitoring of Clonazepam in the clinical first aid and forensic medicine.