摘要
目的：建立梯度洗脱的HPLC法测定葡萄糖酸依诺沙星注射液中有关物质。方法：色谱柱：DiamonsilTMC18（250 mm×4.6 mm,5μm）;流动相A：0.025 mol·L^-1磷酸溶液（三乙胺调pH 3.0）-甲醇-乙腈（80∶10∶10）,流动相B：0.025 mol·L^-1磷酸溶液（三乙胺调节pH 3.0）-甲醇-乙腈（350∶325∶325）,梯度洗脱;流速：1.1 ml·min^-1;检测波长：269 nm、284 nm;进样量：20μl;柱温：40℃。结果：在该色谱条件下,供试品稳定性及分离度良好。5-羟甲基糠醛在19.80 ng·ml^-1-19.80μg·m^l-1范围内与峰面积呈良好的线性关系（r=0.999 9）,检出限为0.18 ng,平均回收率为99.68%,RSD为0.12%（n=9）。结论：本法结果准确、灵敏度高、专属性强、重复性好,可用于葡萄糖酸依诺沙星注射液有关物质的检测。
Objective： To establish a method for the determination of related substances in enoxaein gluconate injection by HPLC with gradient elution. Methods： HPLC was performed on a DiamonsilTM C18 column （250 mm × 4.6 mm, 5 μm） , the mobile phase A was 0.025 mol· L^-1 phosphonic acid solution （adjusting pH to 3.0 with triethylamine）-methanol- acetonitrile （80： 10： 10） and the phase B was 0. 025 mol . L ^- l phosphonic acid solution （ adjusting pH to 3.0 with triethylamine） -methanol-acetonitrile （ 350：325： 325 ） with gradient elution at a flow rate of 1.1 ml · min^-1 , the detection wavelength was 269 nm and 284 nm, the injection volume was 20 μl, and the column temperature was 40℃. Results： Under the HPLC conditions, the samples had good stability and separation. The calibration curve was linear within the concentration range of 19.80 ng · ml^-1-19.80 μg · ml^- 1 （r = 0. 999 9 ） for 5-hydroxymethylfurrural with the detection limit of 0.18ng, and the average recovery was 99.68 % with RSD of 0.12% （n = 9 ）. Conclusion： The method is accurate, sensitive, specific and reproducible, and can be used in the determination of related substances in enoxaein gluconate injection.
出处
《中国药师》
CAS
2015年第6期936-939,共4页
China Pharmacist
