RP-HPLC法同时测定复方酚咖伪麻胶囊5种组分的含量  

Simultaneous determination of five ingredients in compound paracetamol caffeine and pseudoephedrine hydrochloride capsules by RP-HPLC

作　　者：王丽琼 赵雪[2] 刘明容 魏长勇 吴晓燕 

机构地区：[1]乐山市食品药品检验检测中心,乐山614000 [2]乐山职业技术学院,乐山614000

出　　处：《药物分析杂志》2016年第8期1403-1408,共6页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立同时测定复方酚咖伪麻胶囊中5种组分含量的RP-HPLC法。方法:采用XTerra R RP18色谱柱(250 mm×4.6 mm,5μm),以甲醇为流动相A,0.02 mol·L-1磷酸二氢钾溶液-三乙胺(100∶0.02)为流动相B,梯度洗脱,流速1.0 m L·min^(-1),柱温30℃,检测波长215 nm。结果:复方酚咖伪麻胶囊中对乙酰氨基酚、马来酸氯苯那敏、盐酸氯哌丁、盐酸伪麻黄碱和咖啡因的分离度符合要求;线性范围分别为150.55~1 505.49μg·mL^(-1)(r=0.999 7)、1.29~12.90μg·mL^(-1)(r=1.000)、6.03~60.30μg·mL^(-1)(r=0.999 8)、14.95~149.45μg·mL^(-1)(r=0.999 9)和12.62~126.20μg·mL^(-1)(r=0.999 9);平均回收率(n=9)分别为98.9%、98.4%、100.9%、100.1%和100.3%;定量限分别为0.06、0.12、0.07、0.15和0.03μg·mL^(-1);供试品溶液在24 h内稳定,RSD(n=7)分别为0.7%、0.5%、1.3%、0.5%和0.5%;方法耐用性好,在不同柱温(±1℃)条件下,RSD(n=3)分别为0.1%、0.7%、0.2%、0.1%和0.2%,不同流速(±0.01 m L·min^(-1))条件下,RSD(n=3)分别为1.0%、1.7%、1.2%、1.3%和0.7%。3批样品中对乙酰氨基酚、马来酸氯苯那敏、盐酸氯哌丁、盐酸伪麻黄碱和咖啡因的含量分别为96.0%~98.9%、92.4%~97.1%、93.8%~100.3%、95.3%~100.0%和96.7%~99.2%。结论:本法经方法学验证,适用于复方酚咖伪麻胶囊的质量评价。Objective： To establish an RP-HPLC method for simultaneous determination of five ingredients in compound paracetamol caffeine and pseudoephedfine hydrochloride capsules. Methods： The analysis was performed on an XTerra RP18 column （ 250 mm × 4.6 mm, 5μ m ）with gradient elution of methanol and 0.02 mol· L^-1 potassium dihydrogen phosphate-tfiethylamine （ 100 ： 0.02 ） at the flow rate of 1.0 mL· min^-1. The column temperature was 30 ℃, and the detection wavelength was 215 nm. Results： Peaks of paracetamol, chlorphenamine maleate, cloperastinehydrochloride, pseudoephedrine hydrochloride and caffeine were successfully separated from each other. The linear ranges of calibration curves were 150.55-1505.49 μg·mL^-1 （ r=-0.999 7 ）, 1.29-12.90 μg·mL^-1 （ r=-l.000 ）, 6.03- 60.30 μg·mL^-1 （ r=0.999 8 ）, 14.95-149.45 μg·mL^-1 （ r=0.999 9 ） and 12.62-126.20 μg·mL^-1 （ r=-0.999 9 ）, respectively. The average recoveries （n=9）were 98.9%, 98.4%, 100.9%. 100.1% and 100.3%, respectively. The limits of quantification （ LOQs ）were 0.06 μg· mL^-1, 0.12 μg·mL^-1, 0.07 μg·mL^-1, 0.15 μg·mL^-1 and 0.03 μg·mL^-1, respectively. The sample solution was stable within 24 h, the RSDs （ n=7 ） were 0.7%, 0.5%, 1.3%, 0.5% and 0.5%, respectively. The robustness was investigated by varying the conditions of column temperature （ ＋ 1 ~C ） and flow rate（ ＋ 0.01 mL· min^-1 ）, with the RSDs 0.1% and 1.0%, 0.7% and 1.7%, 0.2% and 1.2%, 0.1% and 1.3%, 0.2% and 0.7%, respectively. The contents of paracetamol, chlorphenamine maleate, cloperastine hydrochloride, pseudoephedrine hydrochloride and caffeine in three samples were 96.0%-98.9%, 92.4%-97.1%, 93.8%-100.3%, 95.3%-100.0% and 96.7%-99.2%, respectively. Conclusion： The established method is validated to be suitable for quality control of compound paracetamol caffeine and pseudoephedrine hydrochloride capsules.

关 键 词：复方酚咖伪麻胶囊 对乙酰氨基酚 马来酸氯苯那敏 盐酸氯哌丁 盐酸伪麻黄碱 咖啡因 反相高效液相色谱 梯度洗脱 

分 类 号：R917[医药卫生—药物分析学]