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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。
OBJECTIVE: To identify five effective constituents (Isoborneol, Borneol, Matrine, Sophoridine and Sophocarpine) in Shufu Zhiyang cream by gas chromatography-mass spectrometry (GC-MS) Ion method Simultaneous determination of Shu-Shu anti-itch cream in these five active ingredients analysis. Methods: The samples were alkalified by ammonia water and extracted with ethyl acetate. Methyl salicylate and dioctyl phthalate were used as double internal standard. The samples were separated on a HP-INNOWAX capillary column (30 m × 0.25 mm × 0.25 μm ), The detector is a FID detector, the inlet temperature is 260 ° C, and the detector temperature is 260 ° C. Split injection, split ratio of 10: 1. The temperature was programmed at an initial temperature of 100 ° C for 2 min. The temperature was raised to 250 ° C at 5 ° C min-1 for 20 min. Results: The concentrations of isoborneol, borneol, matrine, sophoridine and sophocarpine in the range of 0.0373-0.0869 mg · mL -1 (r = 0.9997) and 0.0547-0.128 mg · mL -1 (r = 0.9999) (R = 0.9998), 0.0444 ~ 0.133 mg · mL -1 (r = 0.9999), 0.00224 ~ 0.0448 mg · mL -1 (r = 0.9998) and 0.0335 ~ 0.100 mg · mL -1 The average recoveries (n = 9) were 97.8%, 98.0%, 98.4%, 97.8% and 98.1%, respectively. Conclusion: The method is simple, sensitive and accurate. It can be used for the simultaneous determination of isoborneol, borneol, matrine, sophoridine and sophocarpine in Shuisu Zhushi cream.