论文部分内容阅读
目的建立醒脑滴丸及其血浆中右旋龙脑含量的气相色谱(GC)及气相色谱-质谱联用(GC- MS)方法。方法GC法：色谱柱以聚乙二醇(PEG)-20M为固定相,涂布浓度10%,检测器FID,柱温100℃,载气流速1．0 mL/min；GC-MS法：血浆样品用乙醚萃取,选用DB5-MS色谱柱(30 m×0．25 mm×0．25μm),以萘为内标,选择离子检测(右旋龙脑m/z 95,萘m/z 128)。结果GC法：右旋龙脑在0．034～0．102g/L范围内线性关系良好,平均回收率为97．70%(RSD=1．80%)；GC-MS法：右旋龙脑浓度在0．01～20 mg/L范围内线性关系良好,最低检测浓度为3μg/L(S/N＞3),样品平均回收率在91%以上,日内、日间精密度及稳定性的RSD均小于10%。结论两法操作简便、准确、灵敏度高,可作为醒脑滴丸含量测定及其血药浓度分析方法。
Objective To establish GC-GC and GC-MS methods for Xingnao Dripping Pills and its plasma d-bracinolone content. Methods GC method: column with polyethylene glycol (PEG)-20M as stationary phase, coating concentration 10%, detector FID, column temperature 100 °C, carrier gas flow rate 1.0 mL/min; GC-MS method: Plasma samples were extracted with ether and selected on a DB5-MS column (30 m × 0.25 mm × 0.25 μm) with naphthalene as internal standard and selective ion detection (D-brain m/z 95, naphthalene m/z 128 ). Results The GC method showed a good linearity in the range of 0.034-0.102 g/L. The average recovery was 97.70% (RSD=1.80%). GC-MS method: D-brain The concentration was in the range of 0.01-20 mg/L with good linearity. The minimum detection concentration was 3 μg/L (S/N>3). The average recovery of the sample was above 91%, and the intraday and interday precision and stability were good. RSD is less than 10%. Conclusions The two methods are simple, accurate and sensitive, and can be used as the determination of the concentration of Xingnao Dripping Pills and the analysis method of blood drug concentration.