高效液相色谱法测定布林佐胺中对甲苯磺酸异丙酯  

Determination of Isopropyl Toluene-4-sulphonate in Brinzolamide by High Performance Liquid Chromatography

作　　者：江凡[1] 张炎[1] 林晓燕 段秋龙 张虹[1] JIANG Fan;ZHANG Yan;LIN Xiaoyan;DUAN Qiulong;ZHANG Hong(Department of Clinical Pharmacology,Tongji Hospital,Tongji University,Shanghai 200065,China;Shandong Viwit Pharmaceutical Co.,Ltd,Tengzhou 277500,China)

机构地区：[1]同济大学附属同济医院临床药理室,上海200065 [2]山东威智医药工业有限公司,滕州277500

出　　处：《医药导报》2018年第7期882-885,共4页Herald of Medicine

摘　　要：目的建立高效液相色谱法测定布林佐胺中基因毒性杂质对甲苯磺酸异丙酯残留量。方法采用Inertisl ODS-3 C_(18)色谱柱(4.6 mm×250 mm,5μm),缓冲液(取磷酸1.0 m L,加水1 000 m L,三乙胺调p H值至3.0)-乙腈(70∶30)为流动相,流速1.0 m L·min^(-1),柱温30℃,进样量为20μL,波长220 nm。结果布林佐胺中其他杂质不干扰对甲苯磺酸异丙酯的测定,专属性良好;对甲苯磺酸异丙酯检测限浓度为0.008 5μg·m L^(-1),定量限浓度为0.028 4μg·m L^(-1);在0.028 4~1.354μg·m L^(-1)范围内与峰面积线性关系良好(r=0.999);样品测定的重复性良好,RSD=0.66%(n=6);平均加样回收率96.9%,RSD=0.70%(n=9)。结论该方法操作简便、准确、专属性强,可以用于布林佐胺中基因毒性杂质对甲苯磺酸异丙酯残留量的检测。ObjectiveTo establish an HPLC analytical method for determining the genotoxic impurity isopropyl toluene-4-sulphonate in brinzolamide.MethodsThe method was performed on an Inertisl ODS-3 C_（18）（4.6 mm×250 mm,5μm）column.The mobile phase was buffer（1.0 m L phosphoric acid and 1 000 m L water,p H adjusted to 3.0 with triethylamine）-acetonitrile（70∶30）and the flow rate was 1.0 m L·min^-1.The column temperature was 30℃.20μL sample solution was injected into the HPLC system and the detection wavelength was 220 nm.ResultsThe other impurities in brinzolamide did not interfere with the determination of isopropyl toluene-4-sulphonate,which had good specificity.The limit of detection was 0.008 5μg·m L^-1,and the limit of quantification was 0.028 4μg·m L^-1.The calibration curve of isopropyl toluene-4-sulphonate was in a good linearity over the range of 0.028 4-1.354μg·m L^-1（r=0.999）.Determination repetition of isopropyl toluene-4-sulphonate was fine and RSD was 0.66%（n=6）.The average recovery of isopropyl toluene-4-sulphonate was96.9%and RSD was 0.70%（n=9）.Conclusion The method was easy to operate,with acceptable accuracy and specificity,and applicable for the determination of genotoxic impurity isopropyl toluene-4-sulphonate in brinzolamide.

关 键 词：布林佐胺 基因毒性杂质 对甲苯磺酸异丙酯 色谱法 高效液相 

分 类 号：R988.1[医药卫生—药品] R927.1[医药卫生—药学]