HPLC法同时测定市售滴眼液中4种抑菌剂的含量
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篇名: | HPLC法同时测定市售滴眼液中4种抑菌剂的含量 |
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摘要: | 目的:建立同时测定市售滴眼液中羟苯甲酯、羟苯乙酯、羟苯丙酯和苯扎氯铵4种抑菌剂含量的方法。方法:采用高效液相色谱法。色谱柱为Hypersil GOLD C18,流动相为0.005 mol/L醋酸铵溶液(每1 L中含三乙胺10 mL,用冰醋酸调节pH为5.0±0.5)-乙腈(45 ∶ 55,V/V),流速为1.0 mL/min,检测波长分别为262 nm(羟苯甲酯、羟苯乙酯和羟苯丙酯)、214 nm(苯扎氯铵),柱温为30 ℃,进样量为20 μL。结果:羟苯甲酯、羟苯乙酯、羟苯丙酯和苯扎氯铵检测质量浓度线性范围分别为1.235 0~15.438 0 μg/mL(r=0.999 9)、1.317 0~16.383 6 μg/mL(r=0.999 7)、1.207 2~15.089 4 μg/mL(r=0.999 6)、17.776~222.0 μg/mL(r=0.999 9);定量限分别为2.0、2.0、2.0、1.11 μg,检测限分别为0.375、0.375、0.375、0.333 μg;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为98.14%~102.48%(RSD=1.6%,n=9)、98.79%~102.42%(RSD=1.3%,n=9)、98.19%~102.49%(RSD=1.5%,n=9)和98.76%~100.53%(RSD=0.6%,n=9)。结论:该方法结果准确、重复性好、操作简单,适用于市售滴眼液中羟苯甲酯、羟苯乙酯、羟苯丙酯和苯扎氯铵含量的同时测定。 |
ABSTRACT: | OBJECTIVE: To establish a method for simultaneous determination of residual methylparaben, ethylparaben, nipasol and benzalkonium chloride in marketed eye drops. METHODS: HPLC method was adopted. The determination was performed on Hypersil GOLD C18 column with mobile phase consisted of 0.005 mol/L ammonium acetate (10 mL triehtylamine in 1 L solution, pH adjusted to 5.0±0.5 with glacial acetic acid)-acetonitrile (45 ∶ 55,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was 262 nm (methylparaben, ethylparaben, nipasol) and 214 nm (benzalkonium chloride), respectively. The column temperature was 30 ℃ and sample size was 20 μL. RESULTS: The linear range were 1.235 0-15.438 0 μg/mL for methylparaben(r=0.999 9), 1.317 0-16.383 6 μg/mL for ethylparaben (r=0.999 7), 1.207 2-15.089 4 μg/mL for nipasol (r=0.999 6) and 17.776-222.0 μg/mL for benzalkonium chloride (r=0.999 9), respectively. Limits of quantitation were 2.0, 2.0, 2.0, 1.11 μg, respectively; limits of determination were 0.375, 0.375, 0.375, 0.333 μg, respectively. RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The average recoveries were 98.14%-102.48% (RSD=1.6%,n=9), 98.79%-102.42%(RSD=1.3%, n=9), 98.19%-102.49%(RSD=1.5%,n=9) and 98.76%-100.53% (RSD=0.6%,n=9), respectively. CONCLUSIONS: The method is accurate, reproducible, simple and suitable for the determination of residual methylparaben, ethylparaben, nipasol and benzalkonium chloride in marketed eye drops. |
期刊: | 2017年第28卷第15期 |
作者: | 田洁,彭博,吴世杰,赵丽元,邹亮,郝爱鱼,丁红雨 |
AUTHORS: | TIAN Jie,PENG Bo,WU Shijie,ZHAO Liyuan,ZOU Liang,HAO Aiyu,DING Hongyu |
关键字: | 高效液相色谱法;滴眼液;抑菌剂;羟苯甲酯;羟苯乙酯;羟苯丙酯;苯扎氯铵 |
KEYWORDS: | HPLC; Eye drops; Preservatives; Methylparaben; Ethylparaben; Nipasol; Benzalkonium chloride |
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