复方氯化钠滴眼液中羟苯乙酯含量测定及抑菌效力评价

Content Determination of Ethylparaben in Compound Sodium Chloride Eye Drops and Evaluation of Its Bacteriostatic Efficacy

目的建立测定复方氯化钠滴眼液中羟苯乙酯含量的高效液相色谱法,并评价抑菌效力。方法色谱柱为DIKMA Diamonsil C18柱(150 mm×4.6 mm,5μm),流动相为0.05 mol/L磷酸二氢铵溶液(氨水调pH至5.0)-乙腈(60∶40,V/V),流速为1.0 mL/min,检测波长为256 nm,柱温为30℃,进样量为20μL。对含不同质量浓度羟苯乙酯的复方氯化钠滴眼液进行抑菌效力评价。结果羟苯乙酯质量浓度在3.31~105.80μg/mL范围内与峰面积线性关系良好(r=1,n=6);检测限为0.08μg/mL,定量限为0.15μg/mL;精密度、稳定性、重复性试验结果的RSD均低于2.0%(n=6);平均加样回收率为99.81%,RSD为1.42%(n=9)。标示量为0.05~0.5 mg/mL羟苯乙酯的复方氯化钠滴眼液均不能完全达到2020年版《中国药典(四部)》规定的抑菌效力。结论建立的方法可用于复方氯化钠滴眼液中羟苯乙酯的含量测定,应重新对该制剂中抑菌剂的添加量进行评价。

Objective To establish a high-performance liquid chromatography(HPLC)method for the content determination of ethylparaben in Compound Sodium Chloride Eye Drops,and to evaluate its bacteriostatic efficacy.Methods The chromatographic column was Dikma Diamonsil C18 column(150 mm×4.6 mm,5μm),the mobile phase was 0.05 mol/L ammonium dihydrogen phosphate solution(pH 5.0 adjusted by aqueous ammonia)-acetonitrile(60∶40,V/V),the flow rate was 1.0 mL/min,and the detection wavelength was 256 nm,the column temperature was 30℃,and the injection volume was 20μL.The bacteriostatic efficacy of Compound Sodium Chloride Eye Drops containing different concentrations of ethylparaben was evaluated.Results The linear range of ethylparaben was 3.31-105.80μg/mL(r=1,n=6).The limit of detection(LOD)was 0.08μg/mL,and the limit of quantitation(LOQ)was 0.15μg/mL.The RSDs of precision,stability,and repeatability tests were lower than 2.0%(n=6).The average recovery of ethylparaben was 99.81%with an RSD of 1.42%(n=9).Compound Sodium Chloride Eye Drops with a labeled amount of 0.05-0.5 mg/mL ethylparaben could not fully achieve the bacteriostatic efficacy recorded in the Chinese Pharmacopoeia(2020 Edition,VolumeⅣ).Conclusion The established method can be used for the content determination of ethylparaben in Compound Sodium Chloride Eye Drops,and the addition dose of antibacterial agents in this preparation should be re-evaluated.