交联玻璃酸钠注射液中残留交联剂乙烯砜的测定

摘要

Objective To establish a method to quantify the residual cross-linker vinyl sulfone and its hydration product 1 ,4-Thioxane-1 ,1-Dioxide.Methods The polysaccharide was precipitated by ethanol,however vinyl sulfone and its hydration product were soluble,and can be analyzed by direct injection.The analysis was carried on Agilent DB-wax capillary column (30m ×0.53 mm,1.0 μm).The flame ionization detector (FID)and flame photometric detector (FPD)were used to detect samples and the efficiency were compared. Results The linear range of vinyl sulfone and its hydration product were separately 0.5 ~20μg/mL and 2~100μg/mL detected by FID.The Limit of Quantity (LOQ)were 0.8μg/mL and 2.3μg/mL, respctively.The Limit of Detection (LOD)were 2.6μg/mLand 7.6μg/mL,respectively,and the average recoveries (n=9)of them were 104.3%and 92.4%,respectively.Conclusion FID could meet the needs of the test,and this method is simple and accurate with high sensitivity and good repeatability,which can be used for quality control of trace vinyl sulfone and its hydration products 1 ,4-Thioxane-1 ,1-Dioxide in cross-linked sodium hyaluronate injection.%目的：建立交联玻璃酸钠注射液中交联剂乙烯砜和其水化产物1，4-噻恶烷-1，1-二氧残留量的测定方法。方法用乙醇萃取样品，乙烯砜和其水化产物溶于乙醇，玻璃酸钠不溶于乙醇生成白色沉淀，取上清液直接进样，用气相色谱仪分析。色谱柱为Agilent DB-wax（30 m ×0.53 mm，1.0μm）；分别使用氢火焰离子化检测器（flame ionization detector，FID）和火焰光度检测器（flame photometric detector，FPD）进行测定并对比结果。结果 FID测定乙烯砜和其水化产物的线性范围分别为0.5～20μg/mL 和2～100μg/mL；定量限分别为2.6μg/mL和7.6μg/mL；检测限分别为0.8μg/mL和2.3μg/mL；加样回收率分别为104.3％和92.4％。FPD测定结果与FID测定结果差异无统计学意义。结论使用FID已可以满足检验需要，该方法灵敏、快速、专属性强，可用来同时控制产品中痕量的乙烯砜和其主要水化产物1，4-噻恶烷-1，1-二氧。