高效液相色谱-串联质谱法测定中药口服液中23种防腐剂

目的：建立同时测定中药口服液产品中苯甲酸、山梨酸、三氯卡班、4-羟基苯甲酸丙酯、4-羟基苯甲酸异丙酯等23种防腐剂的的高效液相色谱-串联质谱检测方法。方法：样品以甲醇为提取溶剂进行超声提取，离心后取上清液以Acquity UPLC BEH C₁₈色谱柱（2.1 mm×100 mm，1.7 μm）进行分离，0.01 mol·L^-1醋酸铵溶液和甲醇为流动相梯度洗脱；流速为0.4 mL·min^-1。结果：在相应的浓度范围内，23种防腐剂质量浓度与峰面积呈良好的线性关系（r≥0.99）；检测下限在1~40 ng·mL^-1间；平均回收率范围为75.1%~115.0%，日内精密度为0.92%~3.3%。结论：该方法分析速度快，准确度好，灵敏度高，可用于中药口服液中防腐剂的快速筛查。  

Objective:To develop a liquid chromatography tandem mass spectrometry(LC-MS/MS) method for the simultaneous determination of 23 kinds of preservatives in traditional Chinese medicine oral liquid including benzoic acid,sorbic acid,triclocarban,propyl 4-hydroxybenzoate and isopropyl 4-hydroxybenzoate,etc.Methods:The samples were ultrasonically extracted with methanol,then the separation was carried out on an Acquity UPLC BEH C₁₈ column(2.1 mm×100 mm,1.7 μm) with gradient elution of 0.01 mol·L^-1 ammonium acetate aqueous solution and methanol. The flow rate was 0.4 mL·min^-1. Results:The concentration of 23 preservatives showed good linear relationship of peak area and the corresponding concentration(r>0.99). The limits of detection(LODs) were in the range of 1~40 ng·mL^-1. The average recoveries were 75.1%-115.0% and the RSDs of the intraday precisions test were in the range of 0.92%~3.3%. Conclusion:The method is accurate,fast and sensitive,and it is suitable for the rapid screen of 23 kinds of preservatives in traditional Chinese medicine oral liquid. 

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