摘要
目的建立了梯度洗脱高效液相色谱法同时测定磷酸川芎嗪注射剂中苯酚、苯甲醇、对羟基苯甲酸甲酯、三氯叔丁醇、对羟基苯甲酸丙酯等5种常用抑菌剂含量的测定方法。方法采用Alltima C18色谱柱(250 mm×4.6 mm,5μm),以水-甲醇为流动相,梯度洗脱,流速为1.0 mL/min,检测波长:苯酚、苯甲醇、三氯叔丁醇均选择220 nm;对羟基苯甲酸甲酯和对羟基苯甲酸丙酯选择256 nm,柱温30℃。结果苯酚、苯甲醇、对羟基苯甲酸甲酯、三氯叔丁醇、对羟基苯甲酸丙酯分别在线性范围2.12~105.92(r=0.9998)、7.03~351.60(r=0.9999)、0.47~23.60(r=0.9997)、104.12~5206(r=0.9998)、0.59~29.26(r=0.9999)μg/mL范围内线性关系良好,平均加样回收率分别为98.8%、104.5%、97.0%、97.8%、99.0%,RSD分别为1.9%、3.1%、2.8%、2.6%、1.8%(n=9)。114批样品中均未检出抑菌剂。结论本方法简便、准确、专属性强,可用于磷酸川芎嗪注射剂中苯酚、苯甲醇、对羟基苯甲酸甲酯、三氯叔丁醇、对羟基苯甲酸丙酯等抑菌剂的快速筛查与含量测定。
Objective To establish an HPLC method for the determination of Five bacteriostatic Agents(phenol,benzyl alcohol,methyl hydroxybenzoate,Chlorobutanol and Propyl 4-hydroxybenzoate)in Tetramethylpyrazine Phosphate injection.Methods Alltima C18(250 mm×4.6 mm,5μm)was adopted with the mobile phase of water-methyl alcohol,gradient elution,at a flow rate of 1.0 mL·min-1.The detection wavelength for phenol、benzyl alcohol and methyl hydroxybenzoate were set at 220 nm,Chlorobutanol and Propyl 4-hydroxybenzoate at 256 nm.The average recovery rates for phenol,benzyl alcohol,methyl hydroxybenzoate,Chlorobutanol and Propyl 4-hydroxybenzoate were 98.8%,104.5%,97.0%,97.8%,99.0%and RSD 1.9%,3.1%,2.8%,2.6%and 1.8%(n=9).Results The calibration curve of phenol,benzyl alcohol,methyl hydroxybenzoate,Chlorobutanol and Propyl 4-hydroxybenzoate all showed good linear in range of 2.12~105.92(r=0.9998),7.03~351.60(r=0.9999),0.47~23.60(r=0.9997),104.12~5206(r=0.9998),0.59~29.26μg/mL(r=0.9999).Conclusion The method is simplicity,accurate and reproducible,and can control the quality of the preparation effectively,and can be used for the rapid identify or determnation of phenol,benzyl alcohol,methyl hydroxybenzoate,Chlorobutanol and Propyl 4-hydroxybenzoate in Tetramethylpyrazine Phosphate injection.
作者
朱永琴
ZHU Yong-qin(Henan Provincial Institute for Food and Drug Control,Zhengzhou 450018,China)
出处
《医药论坛杂志》
2020年第6期37-40,共4页
Journal of Medical Forum
