GC法同时测定肤舒止痒膏中5个有效成分的含量

GC simultaneous determination of five active ingredients in Fushuzhiyang ointment

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×0.25μm),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。

To identify five active ingredients （ isoborneol, bomeol, matrine, sophoridine, and sopho- carpine） 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 - INNO- WAX 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.