HPLC法测定氨麻美敏片、氨麻美敏片(Ⅱ)和氨麻美敏片(Ⅲ)中4种有效成分的含量

Determination of four active ingredients in three types of Paracetamol,Pseudoephedrine Hydrochloride,Dextromethorphan Hydrobromide and Clorphenamine Maleate Tablets by HPLC

目的:建立测定氨麻美敏片、氨麻美敏片(Ⅱ)、氨麻美敏片(Ⅲ)中对乙酰氨基酚、盐酸伪麻黄碱、氢溴酸右美沙芬和马来酸氯苯那敏含量的方法。方法:采用两套高效液相色谱法。(1)测定对乙酰氨基酚:色谱柱为Agela Venusil XBP C8柱(250 mm×4. 6 mm,5μm),流动相为甲醇-水-冰醋酸(20∶79∶1),检测波长为280 nm,流速为1. 0 ml/min,柱温为40℃,进样量为10μl。(2)测定盐酸伪麻黄碱、氢溴酸右美沙芬和马来酸氯苯那敏:色谱柱为phenomenex Luna Phenyl柱(250 mm×4. 6 mm,5μm),流动相为甲醇-水(60∶40)(每100 ml混合液中含磷酸二氢钾0. 34 g,三乙基氯化铵0. 3 g,十二烷基硫酸钠0. 15 g和磷酸0. 1 ml),检测波长为214 nm,流速为1. 0 ml/min,柱温为40℃,进样量为10μl。结果:(1)对乙酰氨基酚检测质量浓度线性范围为0. 25～1. 00 mg/ml(r=0. 999 9);精密度、稳定性、重复性试验的RSD均<0. 5%;平均回收率为100. 2%(RSD为0. 4%,n=9)(2)盐酸伪麻黄碱、氢溴酸右美沙芬和马来酸氯苯那敏检测质量浓度线性范围分别为36. 20～180. 98μg/ml、17. 99～89. 94μg/ml和2. 41～12. 06μg/ml(r分别为0. 999 9、0. 999 9和0. 999 7);精密度、稳定性、重复性试验的RSD均<0. 5%; 30/15/2规格平均回收率分别为99. 7%、99. 2%和99. 5%,RSD分别为1. 0%、0. 8%和0. 5%(n=9); 30/10/2规格平均回收率分别为99. 4%、99. 5%和100. 0%,RSD分别为0. 9%、0. 6%和0. 6%(n=9)。结论:该方法简单快速,准确性好,可用于控制氨麻美敏片、氨麻美敏片(Ⅱ)、氨麻美敏片(Ⅲ)中4种有效成分的质量。

Objective: To establish a HPLC method for contents determination of the four active ingredients of in three types of paracetamol,pseudoephedrine hydrochloride,dextromethorphan hydrobromide and chlorphenamine maleate tablets.Methods: Two HPLC methods were used for content determination.①The chromatographic conditions for content determination of paracetamol were as follows: Agela Venusil XBP C8 column with the column temperature at 40 ℃; methanol-water-acetic acid (20∶79∶1) as mobile phase with flow rate of 1.0 ml/min; injection volume was 10 μl.Paracetamol was detected by UV detector at wavelength of 280 nm.②For the content determination of pseudoephedrine hydrochloride,dextromethorphan hydrobromide and chlorphenamine maleate,the chromatographic conditions were as follows: Phenomenex Luna Phenyl column was used with the column temperature at 40 ℃; methanol-water (60∶40,containing 0.34 g of potassium dihydrogen phosphate,0.3 g of triethyl ammonium chloride,0.15 g of sodium dodecyl sulfate and 0.1 ml of phosphoric acid in 100 mL mixed solution) as mobile phase with low rate of 1.0 ml/min; injection volume was 10 μl; and the detection wavelength was 214 nm.Results:①The linear range of paracetamol was 0.25~1.00 mg/ml( r=0.9999).RSD values of precision,stability and reproducibility tests were lower than 0.5%,and recovery rate was 100.2%(RSD=0.4%,n=9).② The linear ranges for pseudoephedrine hydrochloride,dextromethorphan hydrobromide and chlorphenamine maleate were 36.20~180.98 μg/ml( r=0.9999),17.99~89.94 μg/ml ( r=0.9999) and 2.41~12.06 μg/ml( r=0.9997),respectively.RSD values of precision,stability and reproducibility tests were lower than 0.5%.Recovery rates for 30/15/2 specification were 99.7%(RSD=1.0%,n=9),99.2%(RSD=0.8%,n=9),99.5%(RSD=0.5%,n=9),respectively ; while for specification 30/10/2 ,the recovery rates were 99.4%(RSD=0.9%,n=9),99.5%(RSD=0.6%,n=9),100.0%(RSD=0.6%,n= 9),respectively.Conclusions: The method established in this paper is simple,rapid and reproducible,which can be applied for the quality control of four active ingredients of three types of Paracetamol,Pseudoephedrine Hydrochloride,Dextromethorphan Hydrobromide and Clorphenamine Maleate Tablets.