摘要
目的建立高效液相色谱法同时测定酒石酸溴莫尼定滴眼液中可能含有的12种常见抑菌剂(苯甲酸、苯甲醇、山梨酸、羟苯甲酯、硫柳汞钠、羟苯乙酯、盐酸氯己定、羟苯丙酯、羟苯丁酯、苯扎氯铵、度米芬、苯扎溴铵)的含量,对收集到的国内4个生产厂家的48批样品进行检测及评价。方法采用资生堂CAPCELL PAK C18 MGII色谱柱(4.6×250 mm,5μm);以0.02 mol/L乙酸铵溶液(用冰醋酸调节pH值至4.5)为流动相A,甲醇为流动相B,梯度洗脱,检测波长为262 nm。结果12种抑菌剂间分离度均符合要求,空白辅料对抑菌剂测定没有干扰,各抑菌剂在所考察的浓度范围内具有良好的线性关系,平均回收率范围为92.8%~105.7%,RSD为0.3%~1.9%(n=9)。结果显示48批样品所测抑菌剂的种类与处方标示相符,抑菌剂含量为各自处方标示量的24%~102%。结论该方法灵敏、快速、专属性强,可作为酒石酸溴莫尼定滴眼液中抑菌剂质量控制的方法,为滴眼液的质量控制提供依据。
Objective To establish an HPLC method for the simultaneous determination of 12 common bacteriostatic agents(benzoic acid,benzyl alcohol,sorbic acid,methylparaben,thimerosal,ethylparaben,chlorhexidine acetate,propyl hydroxybenzoate,butyl p-hydroxybenzoate,benzalkonium bromide,domiphen bromide,benzalkonium chloride)in brimonidine tartrate eye drops.The 48 batches of samples collected from 4 domestic manufacturers were tested and evaluated.Methods Shiseido CAPCELL PAK C18 MGII column(4.6 mm×250 mm,5μm)was used,0.02 mol/L ammonium acetate(pH adjusted to 4.5 by glacial acetic acid)(mobile phase A)and methyl alcohol(mobile phase B)were used for gradient elution,and the detection wavelength was 262 nm.Results The separation degree of 12 bacteriostatic agents reached the requirements,and the blank excipients did not interfere with the determination of bacteriostatic agents,the linear relationship of bacteriostatic agents in their linear range was good,the average recoveries were in the range of 92.8%to 105.7%and the RSDs were 0.3%~1.9%(n=9).The qualitative analysis showed that the types of bacterial inhibitors in 48 batches were all in agreement with the formulation.The quantitative determination showed that the contents of bacterial inhibitors were between 24%~102%of the formulation.Conclusion The method is sensitive,rapid and specific,and can be used for the accurate quantitative determination of multiple bacteriostatic agents in brimonidine tartrate eye drops.This study can provide technical support for the standardized use of bacteriostatic agents in this variety.
作者
蒋静静
JIANG Jing-Jing(Wuxi Center for Drug Safety Control,Wuxi 214028,China)
出处
《实验室检测》
2024年第6期37-42,共6页
Laboratory Testing
关键词
抑菌剂
酒石酸溴莫尼定滴眼液
梯度洗脱
高效液相色谱法
bacteriostatic agents
brimonidine tartrate eye drops
gradient elution
high performance liquid chromatography
