高效液相色谱法测定复方甘草口服溶液中8种防腐剂  

Determination of 8 preservatives in Compound Glycyrrhiza Oral Solution by high performance liquid chromatography

作　　者：曾庆花 黄慧 杨娜 李智明 邓鸣 ZENG Qinghua;HUANG Hui;YANG Na;LI Zhiming;DENG Ming(Guangxi Institute for Food and Drug Control,Nanning 530021,China)

机构地区：[1]广西食品药品检验所,南宁530021

出　　处：《化学分析计量》2022年第7期18-22,共5页Chemical Analysis And Meterage

基　　金：广西药品监督管理局2020年直属单位药品安全科研项目(桂药监科2020–直属)。

摘　　要：建立高效液相色谱法测定复方甘草口服溶液中苯甲醇、苯酚、苯甲酸、山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯8种防腐剂。样品经体积分数为50%的甲醇溶液稀释后,以SHISEIDO CAPCELL MGⅡC_(18)色谱柱(250 mm×4.6 mm,5μm)为分离柱,以乙腈–0.02 mol/L乙酸铵溶液(用冰乙酸调至pH 5.0)为流动相,梯度洗脱,流量为1.0 mL/min,检测波长分别为211 nm(苯甲醇、苯酚)、225 nm(苯甲酸)、256 nm(山梨酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯),柱温为30℃。苯甲醇的质量浓度在8.0~160.0μg/mL范围内,山梨酸的质量浓度在3.0~150.0μg/mL范围内,苯酚、苯甲酸的质量浓度在3.0~300.0μg/mL范围内,对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯的质量浓度在0.5~50.0μg/mL范围内与色谱峰面积线性关系良好,相关系数均不小于0.9997,检出限为0.01~2.0μg/mL。样品加标回收率为98.3%~105.1%,测定结果的相对标准偏差为0.8%~6.5%(n=9)。该方法简便、准确,分离效果好。A method was established for simultaneous determination of benzyl alcohol,phenol,benzoic acid,sorbic acid,methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,propyl p-hydroxybenzoate and butyl p-hydroxybenzoate in Compound Glycyrrhiza Oral Solution by high performance liquid chromatography.The samples were diluted with 50%methanol solution.SHISEIDO CAPCELL MGⅡC_(18) column(250 mm×4.6 mm,5μm)was used as separation column with acetonitrile–0.02 mol/L ammonium acetate(glacial acetic acid was used to adjust pH to 5.0)as the mobile phase,gradient elution,and the flow rate was 1.0 mL/min.The detection wavelength was set at 211 nm for benzyl alcohol and phenol,225 nm for benzoic acid,256 nm for sorbic acid,methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,propyl p-hydroxybenzoate,butyl p-hydroxybenzoate,and the column temperature was 30℃.The mass concentration of benzyl alcohol in the range of 8.0–160.0μg/mL,sorbic acid in the range of 3.0–150.0μg/mL,phenol and benzoic acid in the range of 3.0–300.0μg/mL,methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,propyl p-hydroxybenzoate and butyl p-hydroxybenzoate in the range of 0.5–50.0μg/mL had a good linear relationship with the chromatographic peak area,the correlation coefficients were not less than 0.9997,and the detection limits were 0.01–2.0μg/mL.The recoveries of spiked samples were 98.3%–105.1%,and the relative standard deviations of determination results were 0.8%–6.5%(n=9).The method is simple,accurate with good separation.

关 键 词：高效液相色谱法 复方甘草口服溶液 防腐剂 

分 类 号：O657.7[理学—分析化学]