HPLC同时测定双氯芬酸钠滴眼液中3种抑菌剂的含量
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摘要
目的建立HPLC同时测定双氯芬酸钠滴眼液中羟苯乙酯、硫柳汞和苯扎氯铵含量的方法。方法用十八烷基键合硅胶为填充剂,以1%三乙胺溶液(磷酸调节pH值至3.0)为流动相A,以甲醇为流动相B,进行梯度洗脱;流速1.0 mL·min~(-1),柱温40℃,检测波长254 nm。结果羟苯乙酯在20.58～205.8μg·mL~(-1)、硫柳汞在8.242～82.42μg·mL~(-1)、苯扎氯铵n-C12H25取代物在12.88～128.8μg·mL~(-1)、苯扎氯铵n-C14H29取代物在6.624～66.24μg·mL~(-1)内线性良好(r≥0.999 8),平均回收率为99.3%～102.5%(n=9)。结论该方法简单、准确、重复性好,可用于控制双氯芬酸钠滴眼液中羟苯乙酯、硫柳汞和苯扎氯铵的含量。
OBJECTIVE To establish a method for the simultaneous determination of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops by HPLC. METHODS The C18 column was used as analytical column, with 1% triethylamine solution(phosphoric acid adjusted pH to 3.0) as mobile phase A, and methanol as mobile phase B with gradient elution. The column temperature was kept at 40 ℃. The flow rate was 1.0 mL·min~(-1). The detection wavelength was set at 254 nm. RESULTS Between 20.58-205.8 μg·mL~(-1)(ethyl hydroxybenzoate), 8.424-82.42 μg·mL~(-1)(thiomersal),12.88~(-1)28.8 μg·mL~(-1)(benzalkonium chloride n-C12 H25), 6.624-66.24 μg·mL~(-1)(benzalkonium chloride n-C14 H29), their linearities were good, with their recoveries were between 99.3%~(-1)02.5%(n=9). CONCLUSION The method is simple, accurate and reproducible. It can be used to control the content of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops.
OBJECTIVE To establish a method for the simultaneous determination of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops by HPLC. METHODS The C18 column was used as analytical column, with 1% triethylamine solution(phosphoric acid adjusted pH to 3.0) as mobile phase A, and methanol as mobile phase B with gradient elution. The column temperature was kept at 40 ℃. The flow rate was 1.0 mL·min~(-1). The detection wavelength was set at 254 nm. RESULTS Between 20.58-205.8 μg·mL~(-1)(ethyl hydroxybenzoate), 8.424-82.42 μg·mL~(-1)(thiomersal),12.88~(-1)28.8 μg·mL~(-1)(benzalkonium chloride n-C12 H25), 6.624-66.24 μg·mL~(-1)(benzalkonium chloride n-C14 H29), their linearities were good, with their recoveries were between 99.3%~(-1)02.5%(n=9). CONCLUSION The method is simple, accurate and reproducible. It can be used to control the content of ethyl hydroxybenzoate, thiomersal and benzalkonium chloride in diclofenac sodium eye drops.
引文
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[2]双氯芬酸钠滴眼液(迪菲?)说明书[K].2016.
[3]BAUDOUIN C,LABBE A,LIANG H,et al.Preservatives in eye drops:The good,the bad and the ugly[J].Prog Retin Eye Res,2010,29(4):312-334.
[4]DART J.Corneal toxicity:The epithelium and stroma in iatrogenic and factitious disease[J].Eye,2003,17(8):886-892.
[5]张烁,邱良秀,沈远平.各类滴眼剂对角膜上皮细胞的毒性--组织培养法研究[J].眼科新进展,1999,19(3):58-161.
[6]NING L L.Utility and quality control of antimicrobial preservation of ophthalmic preparation during development[J].Chin Pharm J(中国药学杂志),2007,42(23):1836-1838.
[7]安彦.眼用制剂中抑菌剂的应用与质量控制[J].天津药学,2011,23(1):56-58.
[8]ZHANG S L,HE Y L.Preservative for ophthalmic preparation[J].Food Drug(食品与药品),2010,12(9):343-347.
[9]YANG M,LI X,CHEN H.Simultaneous determination of 9bacterial inhibitors in Naphazoline hydrochloride,Chlorphenamine maleate and Vitamin B12 eye drops by HPLC[J].West China J Pharm Sci(华西药学杂志),2017,32(5):533-537.
[10]XU M J,YANG W F,SHI Y F.Determination of three bacteriostatic agents in Bendazac Lysine Eye drops by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2015,32(11):1370-1373.
[11]LIU H Y,ZHOU M,CHENG Q Z,et al.Quality control of bacterial inhibitor in Timolol Maleate Eye drops[J].Chin Pharm(中国药房),2015,26(7):995-999.
[12]中国药典.二部[S].2015:101.