醒脑滴丸中右旋龙脑含量测定及其体内分析方法研究

Content determination and introcorpored analysis of dextroborneol in Xingnao Gutta Pills

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 find a method for the determination of dextroborneol in Xingnao Gutta Pills and plasma by gas chromatography （GC） and GC-mass spectrometry （GC-MS）. Methods In GC procedure the chromatographic column was PEG-20M （10%）, detector was FID, the column temperature was 100℃, and the flow velocity was 1.0 mL/min. In GC-MS procedure the plasma sample was extracted by diethyl ether, the chromatographic column was DBS-MS （30 m × 0.25 mm × 0.25 μm ） , naphthalene was used as internal standard and ion detector was selected （dextroborneol m/z 95, naphthalene m/z 128）. Results In the GC procedure dextroborneol had a good linear relationship in concentration between 0.034 - 0. 102 g/L, the average recovery was 97.70% （ RSD = 1.80% ）. In the GC-MS procedure dextroborneol had a good linear relationship in concentrations between 0.01 - 20 mg/L, the lowest concentration was 3 μg/L （S/N 〉3 ） and the average recovery was over 91% （all SRD of interday and intra -day were below 10% ）. Conclusion These two methods are accurate, sensitive and easy to be performed, and can be used in the content determination and concentration analysis of medicated plasma of Xingnao Gutta Pills.