气相色谱法同时测定重楼解毒酊中5个成分

Simultaneous determination of five compounds in Chonglou Jiedu Tincture by GC

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.