复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测  

Detection of preservatives in compound Jiegeng Mahuangjian syrup(Ⅱ)

作　　者：朱荣 奉艳花 

机构地区：[1]广西食品药品检验所,南宁530021

出　　处：《药物分析杂志》2018年第1期143-150,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：广西食品药品监督管理局2017年直属单位食品药品安全科研项目计划"药品口服溶液剂中抑菌剂处方合理性评价研究"

摘　　要：目的:建立同时检测防腐剂苯甲酸、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、对羟基苯甲酸丁酯、脱氢乙酸的高效液相色谱法,并应用于复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测。方法:采用CAPCELL MGⅡC_(18)色谱柱(250 mm×4.6 mm,5μm)分离,以0.02 mol·L^(-1)醋酸铵溶液(冰醋酸调pH至4.0)为流动相A,甲醇为流动相B,梯度洗脱,流速为1.0 mL·min^(-1),检测波长为255 nm(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、对羟基苯甲酸丁酯)、308 nm(脱氢乙酸)。结果:各化合物在相应的检测质量浓度范围内线性良好(r>0.999 6);精密度、稳定性试验的RSD<2.0%;平均回收率范围为98.3%~112.9%(n=9)。4家企业共43批样品均未检出山梨酸、对羟基苯甲酸酯类及脱氢乙酸;2家企业样品的苯甲酸含量与处方相符,另外2家的不相符。结论:本方法可用于复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测。Objective：To establish an HPLC method for the simultaneous detection of preservatives（benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate,dehydrogenation acid）,and apply to the detection of preservation in compound Jiegeng Mahuangjian syrup（Ⅱ）.Methods：SHISEIDO CAPCELL MG Ⅱ C18 column（250 mm×4.6 mm,5 μm）was adopted. The mobile phase consisted of 0.02 mol·L^-1 ammonium acetate solution（using glacial acetic acid to adjust p H to 4）-methanol with gradient elution at the flow rate of 1.0 mL·min^-1.The detective wavelength was 255 nm for benzoic acid,sorbic acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate and 308 nm for dehydrogenation acid.Results：The calibration curves of the above-mentioned components were linear in the range of the corresponding concentration.The RSDs of precision and stability test were less than 2.0%.The average recovery ranges were 98.3%-112.9%（n=9）.No sorbic acid,parabens and dehydroacetic acid were detected in 43 batches of samples from 4 enterprises. The benzoic acid content of samples from 2 enterprises was consistent with the prescription and that from the other 2 was not.Conclusion：The method is suitable for the detection of preservative in compound Jiegeng Mahuangjian syrup（Ⅱ）.

关 键 词：中药复方 桔梗麻黄碱糖浆 防腐剂 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 对羟基苯甲酸丁酯 脱氢乙酸 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]