目的: 利用气相色谱-质谱联用仪鉴定出肤舒止痒膏中5个有效成分(异龙脑、龙脑、苦参碱、槐定碱、槐果碱)，并建立气相色谱-氢火焰离子法同时测定肤舒止痒膏中这5个有效成分的分析方法。方法: 样品经氨水碱化后，用乙酸乙酯萃取，以水杨酸甲酯和邻苯二甲酸二辛酯作为双内标，采用HP-INNOWAX毛细管色谱柱(30 m×0.25 mm×0.25 μm)，检测器为FID检测器，进样口温度为260℃，检测器温度为260℃。分流进样，分流比为10∶1。升温程序为初始温度100℃，保持2 min；以5℃·min-1升至250℃，保持20 min。结果: 异龙脑、龙脑、苦参碱、槐定碱、槐果碱浓度分别在0.0373~0.0869 mg·mL-1(r=0.9997)、0.0547~0.128 mg·mL-1(r=0.9999)、0.0444~0.133 mg·mL-1(r=0.9999)、0.00224~0.0448 mg·mL-1(r=0.9998)、0.0335~0.100 mg·mL-1(r=0.9998)质量浓度范围内线性关系良好，平均回收率(n=9)分别为97.8%、98.0%、98.4%、97.8%、98.1%。结论: 该方法简单、灵敏，准确度高，可用于同时测定肤舒止痒膏中的异龙脑、龙脑、苦参碱、槐定碱、槐果碱的含量。
Objective: To identify five active ingredients(isoborneol,bomeol,matrine,sophoridine,and sophocarpine)in Fushuzhiyang ointment by GC-MS,and develop a GC-FID method for the component determination of the five active ingredients. Methods: The sample was extracted with acetic ether after adding ammonium hydroxide.Methylis salicylas and DOP were adopted as double internal standards.The GC was performed on an HP-INNOWAX column(30 m×0.25 mm×0.25 μm)with FID detector.The temperature of injector was 260℃,and the temperature of detector was set at 260℃.The temperature program of column oven was programed as follows:100℃ for 2 min,then increased to 250℃ with the rate of 5℃·min-1,and kept 20 min.The injection split ratio was 10∶1. Results: The calibration curves of isoborneol,bomeol,matrine,sophoridine,and sophocarpine were linear in the concentration range of 0.0373-0.0869 mg·mL-1 (r=0.9997),0.0547-0.128 mg·mL-1 (r=0.9999),0.0444-0.133 mg·mL-1 (r=0.9999),0.00224-0.0448 mg·mL-1(r=0.9998),0.0335-0.100 mg·mL-1(r=0.9998),respectively.The mean recoveries(n=9)were 97.8%,98.0%,98.4%,97.8% and 98.1%,respectively.Conclusion: The method is simple,rapid,accurate,which is suitable for the component determination of bomeol,isoborneol,matrine,sophoridine,and sophocarpine in Fushuzhiyang ointment.
