摘要
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 applie
作者
王昕
王卫
唐素芳
Wang Xin;Wang Wei;Tang Sufang(Tianjin Institute for Drug Control,Tianjin 300070)
出处
《天津药学》
2018年第6期5-10,共6页
Tianjin Pharmacy
关键词
氨麻美敏片
氨麻美敏片(Ⅱ)
氨麻美敏片(Ⅲ)
高效液相色谱法
活性成分
含量测定
Paracetamol
Pseudoephedrine Hydrochloride
Dextromethorphan Hydrobromide and Clorphenamine Maleate Tablets (Ⅰ,Ⅱ and Ⅲ)
HPLC
active ingredients
content determination
