HPLC法同时测定马来酸噻吗洛尔滴眼液中噻吗洛尔和羟苯乙酯的含量

目的：建立同时测定马来酸噻吗洛尔滴眼液中噻吗洛尔和羟苯乙酯含量的HPLC法。方法：采用C₁₈色谱柱（4.6 mm×150 mm，5 μm），以乙腈（B）-0.1%磷酸溶液（A）（1 000 mL，加三乙胺1 mL，用氢氧化钠试液调节pH至3.9）为流动相，梯度洗脱（0~5 min，78% A；5~5.2 min，78% A→55% A；5.2~10 min，55% A；10~11 min，55% A→78% A；11~13 min，78% A），流速1.0 mL·min^-1，检测波长275 nm，柱温35℃，进样量20 μL。结果：噻吗洛尔和羟苯乙酯质量浓度分别在6.07~505.99 μg·mL^-1（r=1.000）和0.37~30.68 μg·mL^-1（r=0.999 9）范围内呈良好的线性关系，平均回收率（n=9）分别为99.8%（RSD=0.8%）和99.8%（RSD=0.9%）。7批样品中噻吗洛尔的含量分别为102.7%、100.4%、99.8%、100.4%、104.1%、98.9%和94.2%，羟苯乙酯的含量分别为0.283、0.286、0.291、0.291、0.434、0.137和0.270 mg·mL^-1。结论：该方法经方法学验证，可用于马来酸噻吗洛尔滴眼液的质量控制。

Objective: To establish an HPLC method for simultaneous determination of timolol and ethylparaben in timolol maleate eye drops.Method: The analysis was performed on a C₁₈ column(4.6 mm×150 mm,5 μm)with a mobile phase consisting of acetonitrile(B)-0.1% phosphoric acid solution(A) (1 mL triethylamine per 1 000 mL,pH was adjusted to 3.9 with used sodium hydroxide solution)using gradient elution(0-5 min,78%A;5-5.2 min,78%A→55%A;5.2-10 min,55%A;10-11 min,55%A→78%A;11-13 min,78%A)at a flow rate of 1.0 mL·min^-1.The detection wavelength was 275 nm,and the column temperature was 35℃,and the injection volume was 20 μL.Results: The linear range of timolol and ethylparaben were 6.07-505.99 μg·mL^-1(r=1.000)and 0.37-30.68 μg·mL^-1(r=0.999 9),respectively.The average recoveries(n=9) were 99.8%(RSD=0.8%)and 99.8% (RSD=0.9%),respectively.In seven batches of samples,the content of timolol were 102.7%,100.4%,99.8%,100.4%,104.1%,98.9% and 94.2%,the content of ethylparaben were 0.283,0.286,0.291,0.291,0.434,0.137 and 0.270 mg·mL^-1.Conclusion: The established method is proved by methodology validation that it can be applied to the quality control of timolol maleate eye drops.

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