串联质谱法检测血清中的左羟丙哌嗪

Determination of Levodropropizine in Serum by Tandem Gas Chromatography Mass Spectrometry

血清样品调节成碱性后 ,加到硅藻土小柱上 ,用二氯甲烷洗脱左旋羟丙哌嗪 ,在微弱氮气流下吹干洗脱液 ,残渣以BSTFA衍生后用GC/MS进行定性定量分析 .以m/z 175为母离子 ,子离子质量扫描范围为m/z 5 0～ 2 0 0 ,外标法定量 .方法的线性范围为 :0 .0 0 5～ 4.0 μg/mL ,相关系数为 0 .99,检测低限为 0 .0 0 5mg/L ,回收率范围为 80 %～ 10 2 .5 % ,相对标准偏差范围为 1.6 7%～ 4.0 0 % .

Serum sample was made alkaline by sodium hydroxide, and then was added to minicolumn. Levodropropizine was eluted with methylene dichloride. The eluted organic phase was dried under nitrogen. The residue was derived by BSTFA before analyzed by Tandem GC MS. The parent ion was m/z 175, and daughter ion was from m/z 50 to m/z 200. The external standard method was used for quantitative. The liner range, the correlation coefficient, the detection limit, the recoveries and RSD was 0.005～4.0 μg/mL, 0.99, 0.005 mg/L, 80%～102.5%,1.67 %～4.00 %, respectively.