气相色谱法同时测定麝香止痛贴膏中冰片、薄荷脑和水杨酸甲酯含量

Simultaneous Determination of Borneol,Menthol and Methyl Salicylate in Shexiang ZhitongPlaster by GC

目的 建立同时测定麝香止痛贴膏中冰片、薄荷脑和水杨酸甲酯含量的气相色谱内标法。方法 色谱柱为PEG-20M毛细管柱(30 m×0.32 mm,0.25μm),检测器为氢火焰离子化检测器(FID),以萘为内标,进样口温度为230℃,检测器温度为250℃,程序升温(初始温度100℃、保持15 min,以10℃/min的速率升至200℃、保持5 min),进样量为1μL,分流比为5∶1。结果 冰片、薄荷脑、水杨酸甲酯的质量浓度分别在0.078 6~1.572 5 ng/mL、0.124 9~2.498 4 ng/mL、0.080 0~1.606 0 ng/mL范围内与对照品和内标峰面积比值线性关系良好(r≥0.999 8,n=6);精密度、稳定性、重复性试验的RSD均低于2.0%;加样回收率分别为95.83%,95.01%,95.46%,RSD分别为0.57%,0.34%,0.29%(n=6)。结论 该方法稳定性和重复性均良好,可有效控制麝香止痛贴膏的质量。

Objective To establish a gas chromatography(GC)internal standard method for the simultaneous determination of borneol,menthol and methyl salicylate in Shexiang Zhitong Plaster.Methods The chromatographic column was PEG-20M capillary column(30 m×0.32 mm,0.25μm),the detector was a flame ionization detector(FID),with naphthalene as the internal standard,the inlet temperature was 230℃,the detector temperature was 250℃,the temperature was programmed(the initial temperature was 100℃,maintained for 15 min,and rising to 200℃at the rate of 10℃/min,maintained for 5 min),the injection volume was 1μL,and the split ratio was 5∶1.Results The linear ranges of borneol,menthol and methyl salicylate were 0.0786-1.5725 ng/mL,0.1249-2.4984 ng/mL and 0.0800-1.6060 ng/mL respectively(r≥0.9998,n=6).The RSDs of precision,stability and repeatability tests were all lower than 2.0%.The recovery rates of borneol,menthol and methyl salicylate were 95.83%,95.01%and 95.46%respectively,with the RSDs of 0.57%,0.34%and 0.29%respectively(n=6).Conclusion The method is stable and repeatable,which can effectively control the quality of Shexiang Zhitong Plaster.