HPLC同时测定盐酸萘甲唑啉滴鼻液中9种抑菌剂

Simultaneous Determination of 9 Bacteriostats in Naphazoline Hydrochloride Nasal Drops by HPLC

关键词:  抑菌剂  硫柳汞  苯扎溴铵  羟苯乙酯  苯甲酸钠  盐酸萘甲唑啉滴鼻液  鼻用制剂  高效液相色谱法

Key words:  bacteriostat  thimerosal  benzalkonium bromide  ethyl hydroxybenzoate  sodium benzoate  naphazoline hydrochloride nasal drops  nasal preparation  HPLC

摘要:

目的 建立HPLC同时测定盐酸萘甲唑啉滴鼻液中4类9种常见抑菌剂硫柳汞、羟苯乙酯、苯甲酸钠、羟苯甲酯、羟苯丙酯、羟苯丁酯、山梨酸钾、苯扎氯铵和苯扎溴铵的含量。方法 采用Ultimate XB-C₁₈（4.6 nm×250 nm，5 μm）色谱柱；以乙腈（A）-0.1 mol·L^-1磷酸二氢钠（磷酸调pH 3.7）为流动相，梯度洗脱，流速1.0 mL·min^-1，柱温35℃，检测波长222 nm，样品温度5℃。结果 9种抑菌剂可完全分离，平均回收率为98.2%~100.6%，RSD为0.5%~1.5%。30批样品中检出硫柳汞、羟苯乙酯、苯扎溴铵和苯甲酸钠4种抑菌剂。结论 该法可用于盐酸萘甲唑啉滴鼻液中抑菌剂的质量控制。

Abstract:

OBJECTIVE To establish an HPLC method for simultaneous determination of 4 categories and 9 species common bacteriostats which might be added into naphazoline hydrochloride nasal drops, including thimerosal, ethylparaben, sodium benzoate, methylparaben, propylparaben, butylparaben, sorbic acid, benzalkonium chloride, benzalkonium bromide. METHODS The analysis was performed on Ultimate XB-C₁₈ column(4.6 mm×250 mm, 5 μm) at 35℃, eluted with a gradient program using acetonitrile(A)-0.1 mol·L^-1 sodium phosphate monobasic(pH was adjusted to 3.7 with phosphoric acid) as the mobile phase. The flow rate was 1.0 mL·min^-1, the detection wavelength was 222 nm, and sample was stored at 5℃. RESULTS Under the above conditions, 9 bacteriostats were separated completely. The average recoveries of the 9 components were between 98.2%-100.6%, with RSDs of 0.5%-1.5%. The contents of thimerosal, benzalkonium bromide, ethylparaben and sodium benzoate were detected in 30 batches of naphazoline hydrochloride nasal drops. CONCLUSION The method is suitable to evaluate the quality of bacteriostats in naphazoline hydrochloride nasal drops.