摘要
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.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2013年第11期1882-1886,共5页
Chinese Journal of Pharmaceutical Analysis
关键词
肤舒止痒膏
气相色谱法
龙脑
异龙脑
苦参碱
槐定碱
槐果碱
双内标
Fushuzhiyang ointment
GC
borneol
isoborneol
matrine
sophoridine
sophocarpine
double internal standard