HPLC法测定伏立康唑冻干眼用制剂中的有关物质  

Determination of related substances in voriconazole freeze-dried ophthalmic preparation by HPLC

作　　者：段玺玉 刘小舟[1] 李琳[1] 刘家鑫[1] 于治国[1] 赵云丽[1] 

机构地区：[1]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2016年第12期958-964,共7页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立伏立康唑冻干眼用制剂中有关物质的检查方法。方法采用RP-HPLC法,色谱柱为Thermo Hypersil GOLD C18(250 mm×4.6 mm,5μm);检测波长为256 nm;柱温为35℃;进样量为20μL;流速为1.0 m L·min-1,以甲醇-乙腈-水为流动相,梯度洗脱。结果伏立康唑及各杂质均能得到良好的分离。伏立康唑、杂质A、C和EPC在0.25~5.0 mg·L^(-1)内,杂质D在0.5~2.0 mg·L^(-1)内线性关系良好(r>0.999 0,n=6)。伏立康唑、杂质A、C和EPC质量浓度为2.5 mg·L^(-1),杂质D质量浓度为1.0 mg·L^(-1)时,精密度(RSD)分别为1.3%、1.6%、1.5%、1.3%和1.3%;杂质A、C、D和EPC平均回收率分别为101.2%、101.3%、96.6%和96.6%。经对供试品测定,除杂质D未检出外,其余杂质A、C和EPC峰面积RSD分别为0.02%、0.01%和1.2%。结论该方法适用于伏立康唑冻干眼用制剂的有关物质检查。Objective To develop a method for determination of the related substances in voriconazole freezedried ophthalmic preparation. Methods A high performance liquid chromatography was adopted. The separation was performed on Thermo Hypersil GOLD C18（ 250 mm × 4. 6 mm,5 μm）; detection wavelength was 256 nm; column temperature was 35 ℃; injection volume was 20 μL; the mobile phase consisted of water,methanol and acetonitrile was used as gradient elution for separation with HPLC at a flowrate of1. 0 m L·min- 1. Results Voriconazole and the impurities could get good separation,There were good linear relationships for voriconazole,impurity A,C,EPC at the range of 0. 25- 5. 0 mg·L^-1,and for impurity D at the range of 0. 5- 2. 0 mg·L^-1（ r〉 0. 999,n = 6）. Precision（ RSD） was 1. 3%,1. 3%,1. 5%,1. 6%,and1. 3%,respectively. The recoveries were 102. 3%,101. 3%,101. 2% and 96. 6%,respectively. The repeatability was 1. 20%,0. 01%,0. 02%（ impurity D was not detected）. The samples were stable at 4 ℃for 24 h. Conclusions The method is simple,sensitive and accurate. It could be used for examination of the related substances in voriconazole freeze-dried ophthalmic preparation.

关 键 词：伏立康唑 有关物质 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]