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机构地区:[1]辽宁医学院药学院,锦州121001
出 处:《药物分析杂志》2012年第9期1559-1563,共5页Chinese Journal of Pharmaceutical Analysis
摘 要:目的:建立以毛细管气相色谱同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯含量的方法。方法:采用SE-30(30.0 m×0.25 mm×0.25μm)色谱柱;以正十二烷为内标;柱温采用程序升温:起始温度120℃,保持5 min,以10℃.min-1升温至160℃,保持5 min,再以10℃.min-1升温至240℃,保持5 min;气化温度:260℃;检测器温度:280℃;载气为氮气,流速为3.0 mL.min-1;进样量为1μL,分流比为30∶1。结果:在选定的条件下,乙酸龙脑酯、百秋李醇、去氢木香内酯浓度分别在0.029~1.164 mg.mL-1(r=0.9999)、0.045~1.613 mg.mL-1(r=0.9999)、0.037~1.339 mg.mL-1(r=0.9995)范围内,各成分浓度与内标浓度的比值与其相应的峰面积比值呈良好的线性;平均回收率(n=9)分别为99.7%,99.5%,99.3%。结论:该方法简便准确,重复性好,可用于同时测定沉香化气丸中乙酸龙脑酯、百秋李醇、去氢木香内酯的含量。Objective: To develop a GC method for the determination of bornyl acetate, patchouli alcohol, de- hydrocostus lactone in Chenxiang Huaqi pills. Methods: The GC was performed on a SE -30 capillary column (30. 0 m × 0. 25 mm × 0. 25 m) with an FID detector, and n- dodecane was adopted as the internal standard. The temperature program of column was set as follow: the initial temperature was 120 ℃ and kept for 5 minutes, then increased to 160℃ at a rate of 10 ℃. min-1 and maintained for 5 minutes, after that the temperature would rise to at 240℃ by 10 ℃. min 1, held for another 5 minutes. The injector temperature was 260 ℃ and detector temperature was set at 280 ℃ Nitrogen was used as carrier gas at the flow rate of 3.0 mL .min-1 The injection volume was 1 μL, and injection split ratio was 30: 1. Results: Under certain chromatogram condition, the calibra- tion curves of bornyl acetate, patchouli alcohol and dehydrocostus lactone were linear in the concentration range of 0. 029 - 1. 164 mg. mL-l(r =0. 9999), 0. 045 - 1. 613 mg. mL-1(r =0. 9999), and 0. 037 - 1. 339 mg. mL-1 ( r = 0. 9995 ), respectively. The average recoveries ( n = 9 ) were 99.7 %, 99.5 %, and 99.3 %. Conclusion : The method is simple, accurate, and reproducible, which is suitable for the component determination of bornyl acetate, patchouli alcohol, dehydrocostus lactone in Chenxiang Huaqi pills.
关 键 词:毛细管气相色谱法 沉香化气丸 乙酸龙脑酯 百秋李醇 去氢木香内酯 非极性化合物 中成药含量测定 正十二烷内标
分 类 号:R917[医药卫生—药物分析学]
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