SPE/GC-MS法检测全血中的杜冷丁

Determination of Dolantin in Whole Blood by SPE/GC-MS

建立SPE/GC-MS方法测定全血中杜冷丁的含量。采用MCX 3 mL（60 mg）固相萃取小柱萃取血中杜冷丁,用气相色谱质谱联用仪检测,结合保留时间和特征离子及数据库进行定性和定量分析。杜冷丁在1-20μg/mL范围内线性良好,仪器方法的检出限为0.01μg/mL（S/N≥3）,平均萃取回收率为83.81%,精密度为3.8%,前处理pH值在2-9范围内都能取得良好的萃取效果,C18和HLB固相萃取小柱的对杜冷丁萃取回收率均能达到80%。固相萃取方法适用于全血中杜冷丁的定性定量分析。

An analytical method based on SPE/GC-MS was established for the quantitation of dolantin in whole blood. Dolantin was extracted from blood with solic phase extraction column MCX 3 mL （60 mg）, detected by gas chromatography mass spectrometry, and confirmed by retention time, characteristic ions and NIST database. The extraction was quantified by external standard method. There was good linearity between 1 - 20 μg/mL. The MDL of dolantin was 0. 01μg/mL（S/N≥3）. The recovery of the extraction was about 83.8% and RSD was about 3.8%. When the pH value of buffer solution was between 2 - 9, the extraction effect was good as well. The effect of C18 and HLB SPE columns were above 80%. The method of SPE is applicative to confirm and quantify dolantin in whole blood.