摘要
目的 建立气相色谱(GC)同时定量测定重楼解毒酊(重楼、石菖蒲、艾叶、艾片等)中1,8-桉叶素、樟脑、龙脑、β-细辛醚、α-细辛醚5个有效成分的方法.方法 重楼解毒酊无水乙醇液采用GC法分析,HP-INNOWAX(30 m×0.25 mm ×0.25 μm)色谱柱,升温程序为初始温度60℃保持5 min,以5℃/min升至120℃保持5 min,再以5℃/min升高至180℃保持10 min,最后以20℃/min升至240℃,保持3 min;进样口温度250℃,体积流量1.5 mL/min;分流比5∶1;FID检测器,检测器温度250℃;载气为氮气.结果 1,8-桉叶素、樟脑、龙脑、β-细辛醚和α-细辛醚分别在0.001 48~0.008 85 mg/mL(r=0.999 8),0.002 40 ~0.0192 mg/mL (r=0.9996),0.182 ~1.238 mg/mL(r=0.999 7),0.027 6 ~0.193 mg/mL(r=0.999 9),0.001 26 ~0.010 0 mg/mL(r=0.999 9)范围内线性良好;加样回收率(n=9)分别为96.9% (RSD =1.0%),99.5% (RSD =0.9%),98.6% (RSD =0.9%),96.8% (RSD=2.0%)和99.2% (RSD=0.7%).结论 本方法四阶程序升温方法效果最佳,能满足5个成分同时测定.
AIM To develop a gas chromatography for determining the contents of 1,8-cineole, camphor, bor- neol, β-asarone, α-asarone in Chonglou Jiedu Tincture (Paridis Rhizoma , Acori tatarinowii Rhizoma , Artemisiae argyi Folium, l-borneolum , etc. ). METHODS The anhydrous alcoholic extract of sample was determined on HP-INNOWAX (30 m×0.25 mm ×0.25 μm) capillary column. The temperature programming worked first at 60℃ for 5 min, increased to 120 ℃ at the rate of 5℃/min, and kept 5 min, and then increased to 180 ℃/min at the rate of 5℃/min and held for 10 rain, finally increased to 240℃ at the rate of 20 ℃/min and kept 3 rnin. The injector temperature was set at 250 ℃, the flow rate was 1.5 mL/min, split injection was conducted with split ratio of 5 : 1. FID detector temperature was at 250℃. Nitrogen was used as carrier gas. RESULTS 1,8-Cine- ole, camphor, borneol, β-asarone and α-asarone had good linearity in the ranges of 0. 001 48 - 0. 008 85 mg/mL (r =0. 999 8), 0. 002 40 -0. 019 2 mg/mL (r =0. 999 6), 0. 182 - 1. 238 mg/mL (r =0. 999 7), 0. 027 6 - 0. 193 mg/mL ( r = 0. 999 9 ), 0. 001 26 - 0. 010 0 mg/mL ( r = 0. 999 9 ) and the average recoveries ( n = 9 ) were 96.9% ( RSD = 1.0% ), 99.5% (RSD = 0.9% ), 98.6% ( RSD = 0. 9% ), 96. 8% ( RSD = 2.0% ) and 99.2% ( RSD = 0. 7% ) , respectively. CONCLUSION The developed four-stage programming temperature cansatisfy the determination of five constituents with good precision and accuracy.
出处
《中成药》
CAS
CSCD
北大核心
2014年第10期2091-2094,共4页
Chinese Traditional Patent Medicine
基金
国家科技支撑计划项目(2011BAI13B04-01)
贵州省科技厅科学技术基金(黔科合J字[2011]2275号)
贵州省优秀科技教育人才省长专项资金(2005)297