目的:建立同时测定滴眼剂中羟苯酯类和季铵盐类抑菌剂含量的通用型方法.方法:采用Agilent C18色谱柱(4.6 mm ×250 mm,5 μm),以1％三乙胺溶液(用磷酸调pH至5.0)为流动相A,以甲醇为流动相B,梯度洗脱,柱温为40℃;检测波长为214 nm,流速为1 mL·min-1,进样体积20 μL.结果:羟苯甲酯、羟苯乙酯、羟苯丙酯、羟苯丁酯、苯扎氯铵及苯扎溴铵分别在0.11～559.0、0.10～513.0、0.10～258.8、0.11～270.5、1.07～537.0及1.03～512.8μg·mL-1范围内线性关系良好(r＞0.999),羟苯乙酯、苯扎溴铵、苯扎氯铵的平均加样回收率分别为 104.7％(RSD=1.3％)、102.6％(RSD=1.1％)、100.9％(RSD=1.1％).对12家企业36个品种的100批次滴眼液中抑菌剂含量进行测定,得到了较为准确的结果.结论:本法可为滴眼剂中抑菌剂含量测定质量控制和安全评价提供参考.
Abstract
Objective:To establish a general method for the simultaneous determination of hydroxyphenyl esters and quaternary ammonium bacteriostatic agents in eye drops.Methods:The chromatographic analysis was per-formed on an Agilent C18 column(4.6 mm ×250 mm,5 μm)with 1％triethylamine solution(pH adjusted to 5.0 with phosphoric acid)as mobile phase A and methanol as mobile phase B.Gradient elution was performed at col-umn temperature of 40 ℃.The detection wavelength was 214 nm,the flow rate was 1 mL·min-1,and the injec-tion volume was 20 μL.Results:Methylparaben,ethylparaben,propylparaben,butylparaben,benzalkonium chlo-ride and benzalkonium bromide were 0.11-559.0,0.10-513.0,0.10-258.8,0.11-270.5,1.07-537.0 and 1.03-512.8 μg·mL-1,respectively.The linear range was good(r＞0.999).The average recoveries of meth-ylparaben,benzalkonium bromide and benzalkonium chloride were 104.7％(RSD=1.3％),102.6％(RSD=1.1％)and 100.9％(RSD=1.1％),respectively.The contents of bacteriostatic agent in 100 batches of eye drops from 36 varieties of 12 enterprises were determined,and the accurate results were obtained.Conclusion:This meth-od provides a reference for the content quality control and safety evaluation of bacteriostatic agents in eye drops.
维普
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