目的: 采用GC法同时测定琥珀止痛膏中樟脑、薄荷脑、冰片、八角茴香油、桂皮醛和丁香酚的含量,以评价琥珀止痛膏的质量。 方法: 采用毛细管色谱柱Restek Rtx-WAX(30 m×0.25 mm×0.25 μm);程序升温: 起始温度90 ℃,保持2 min后以3 ℃·min-1升至140 ℃,保持6 min,再以7 ℃·min-1升至180 ℃,保持5 min;进样口温度200 ℃;检测器温度250 ℃。 结果: 在同一色谱条件下,樟脑、薄荷脑、冰片(龙脑和异龙脑)、八角茴香油、桂皮醛和丁香酚进样浓度分别在0.168~1.68、0.120~1.20、0.202~2.02、0.248~2.48、0.0720~0.720、0.168~1.68 mg·mL-1范围内呈良好的线性关系;平均加样回收率(n=6)分别为99.9%(RSD=1.3%)、99.7%(RSD=1.8%)、100.0%(RSD=2.1%)、104.0%(RSD=2.0%)、103.4%(RSD=2.8%)和99.3%(RSD=2.0%)。 结论: 本试验为琥珀止痛膏的分析提供了一种准确可靠的检测方法。
Objective: To develop a GC method to determine camphor,menthol,borneol,star anise oil,cinnamic aldehyde and eugenol in Hupo Zhitong plaster. Methods: The GC system consisted of a quartz capillary column Restek Rtx-WAX(30 m×0.25 mm×0.25 μm).The temperature programing rose from 90 ℃(2 min) to 140 ℃ by 3 ℃·min-1,lasting 6 min,then 7 ℃·min-1 to 180 ℃,lasting 5 min in the end.The temperature of the entrance of the capillary vessel column was 200 ℃,and the temperature of the detector was 250 ℃. Results: Under the same chromatogram condition,there was linear relation among camphor,menthol,borneol (borneol and isoborneol),star anise oil,cinnamic aldehyde and eugenol in the range of 0.168-1.68,0.120-1.20,0.202-2.02,0.248-2.48,0.0720-0.720,0.168-1.68 mg·mL-1,respectively.The average recoveries(n=6) were 99.9%,99.7%,100.0%,104.0%,103.4%,99.3%,respectively,and RSDs were 1.3%,1.8%,2.1%,2.0%,2.8%,2.0%,respectively. Conclusion: This experiment provides an accurate and reliable method to control the quality of Hupo Zhitong plaster.