复方麝香雪莲柳酯贴膏中4种挥发性成分含量测定方法的建立
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篇名: 复方麝香雪莲柳酯贴膏中4种挥发性成分含量测定方法的建立
TITLE: Establishment of a method for the determination of four volatile components in Compound shexiang xuelian liuzhi plaster by GC
摘要: 目的 建立同时测定复方麝香雪莲柳酯贴膏中樟脑、薄荷脑、冰片、水杨酸甲酯含量的方法。方法以乙酸乙酯回流提取制备供试品溶液,采用气相色谱法测定。以ShimadzuSH-Rtx-Wax毛细管柱为色谱柱,以火焰离子化检测器为检测器,检测器温度、进样口温度均为200℃,载气(氮气)流速为2.0mL/min,分离比为20∶1,进样量为1.0μL。结果樟脑、薄荷脑、冰片(以异龙脑、龙脑总和计)、水杨酸甲酯检测质量浓度的线性范围分别为11.5~230.4、10.6~211.6、11.3~225.5、11.0~219.1μg/mL(r>0.999),精密度、重复性、稳定性(48h)试验的RSD均小于4%;4种成分的平均加样回收率分别为100.7%、99.7%、98.9%、100.7%(RSD分别为4.3%、2.9%、2.2%、3.7%,n=9)。2种规格的麝香雪莲柳酯贴膏中樟脑、薄荷脑、冰片、水杨酸甲酯的含量分别为16.8~19.5、4.6~6.0、9.8~11.9、6.9~8.2mg/片(7cm×10cm/片)和8.3~8.6、2.2~2.4、4.7~4.8、3.2~3.6mg/片(5cm×7cm/片)。结论成功建立了同时测定复方麝香雪莲柳酯贴膏中4种挥发性成分含量的方法。
ABSTRACT: OBJECTIVE To establish a method for simultaneously determining the contents of camphor ,menthol,borneol and methyl salicylate in Compound shexiang xuelian liuzhi plaster . METHODS The test solution was prepared by reflux extraction with ethyl acetate ,and was determined by gas chromatography (GC). A Shimadzu SH -Rtx-Wax capillary column was used as the chromatographic column ,and a flame ionization detector was used as the detector . The detector temperature and the injector temperature were both set at 200 ℃. The flow rate of carrier gas (nitrogen)was 2.0 mL/min,the separation ratio was 20∶1,and the sample size was 1.0 μL. RESULTS The linear ranges of camphor ,menthol,borneol(calculated by the sum of isoborneol and borneol)and methyl salicylate were 11.5-230.4,10.6-211.6,11.3-225.5,11.0-219.1 μg/mL(r>0.999). RSDs of the precision , repeatability and stability (48 h)tests were all less than 4%. The average recoveries of the four components were 100.7%,99.7%, 98.9% and 100.7%(RSDs were 4.3%,2.9%,2.2%,3.7%,n=9). The contents of camphor ,menthol,borneol and methyl salicylate in two specifications of Compound shexiang xuelian liuzhi plaster were 16.8-19.5,4.6-6.0,9.8-11.9,6.9-8.2 mg/piece(7 cm×10 cm/piece),and 8.3-8.6,2.2-2.4,4.7-4.8,3.2-3.6 mg/piece (5 cm×7 cm/piece). CONCLUSIONS The method is successfully established for simultaneous determination of four volatile components in Compound shexiang xuelian liuzhi plaster .
期刊: 2022年第33卷第20期
作者: 周钢,单莲莲,马方圆,柴冰阳,雷慧兰,陶虹,严华
AUTHORS: ZHOU Gang,SHAN Lianlian,MA Fangyuan,CHAI Bingyang,LEI Huilan,TAO Hong,YAN Hua
关键字: 复方麝香雪莲柳酯贴膏;樟脑;薄荷脑;冰片;水杨酸甲酯;气相色谱法;含量测定
KEYWORDS: Compound shexiang xuelian liuzhi plaster ;camphor;menthol;borneol;methyl salicylate ;gas chromatography ;
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