摘要
目的建立同时测定川贝枇杷糖浆中苯甲酸钠、对苯二酚、脱氢乙酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯和山梨酸等8种防腐剂的高效液相色谱分析方法。方法采用Inertsil ODS-3C_(18)柱(4.6 mm×250 mm,5μm)进行分离,以甲醇-0.02 mol·L^(-1)乙酸铵(含体积分数0.1%的乙酸)溶液为流动相梯度洗脱,流速为1.0 mL·min^(-1),分别在227 nm波长下检测苯甲酸钠、对苯二酚和脱氢乙酸,256 nm波长下检测对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯和山梨酸。结果在相应的浓度范围内,8种防腐剂质量浓度与峰面积呈良好的线性关系(r≥0.999);精密度和稳定性试验RSD<1.7%,平均回收率范围为96.3%~103.3%,RSD为1.6%~2.8%。结论该方法分析速度快,准确度好,可用于中药糖浆剂中防腐剂快速筛查。
Objective To establish an HPLC method for the simultaneous detection of preservatives(sodium benzoate,hydroquinone,dehydrogenation acid,methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate,sorbic acid),and apply to the detection of preservation in Chuanbei Pipa syrup.Methods Inertsil ODS-3 C_(18) column(4.6 mm×250 mm,5μm)was adopted.The mobile phase consisted of methanol-0.02 mol·L^(-1)ammonium acetate solution(containing 0.1%glacial acetic acid)with gradient elution at the flow rate of 1.0 mL·min^(-1).The detective wavelength was 227 nm for sodium benzoate,hydroquinone,dehydrogenation acid and 256 nm for methylparaben,ethylparaben,propylparaben,butyl-p-hydroxybenzoate,sorbic acid.Results The concentration of 8 preservatives showed good linear relationship of peak area and the corresponding concentration(r≥0.999).The RSDs of precision and stability test were less than 1.7%.The average recoveries were 96.3%-103.3%(n=3)and the RSDs were in the range of 1.6%-2.8%.Conclusion The method is simple,accurate and fast,and it is suitable for the rapid screen of 8 kinds of preservatives in traditional Chinese medicine oral liquid.
作者
马永青
杜高锋
李小盼
MA Yongqing;DU Gaofeng;LI Xiaopan(Hebei Institute for Drug and Medical Device Control,Shijiazhuang 050200,China;Hebei Center for Drug Evaluation(Hebei Center for Medical Device Evaluation),Shijiazhuang 050200,China;Chengde Center for Development and Protection of Intellectual va Rights,Chengde 067000,China)
出处
《沈阳药科大学学报》
CAS
CSCD
北大核心
2022年第12期1439-1446,共8页
Journal of Shenyang Pharmaceutical University
