复方桔梗麻黄碱糖浆(Ⅱ)中防腐剂的检测

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 MGⅡ C₁₈色谱柱（250 mm&#215;4.6 mm，5 μm）分离，以0.02 mol&#183;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&#183;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 MGⅡ C₁₈ column(250 mm&#215;4.6 mm,5 μm)was adopted. The mobile phase consisted of 0.02 mol&#183;L^-1 ammonium acetate solution(using glacial acetic acid to adjust pH to 4)-methanol with gradient elution at the flow rate of 1.0 mL&#183;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).