中国生化药物杂志
中國生化藥物雜誌
중국생화약물잡지
CHINESE JOURNAL OF BIOCHEMICAL PHARMACEUTICS
2014年
4期
171-174
,共4页
交联玻璃酸钠%乙烯砜%乙烯砜水化物%1,4-噻恶烷-1,1-二氧%气相色谱法
交聯玻璃痠鈉%乙烯砜%乙烯砜水化物%1,4-噻噁烷-1,1-二氧%氣相色譜法
교련파리산납%을희풍%을희풍수화물%1,4-새악완-1,1-이양%기상색보법
cross-linked sodium hyaluronate injection%vinyl sulfone%hydration product of vinyl sulfone%1,4-Thioxane-1,1-Dioxide%Gas Chromatography
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。
目的:建立交聯玻璃痠鈉註射液中交聯劑乙烯砜和其水化產物1,4-噻噁烷-1,1-二氧殘留量的測定方法。方法用乙醇萃取樣品,乙烯砜和其水化產物溶于乙醇,玻璃痠鈉不溶于乙醇生成白色沉澱,取上清液直接進樣,用氣相色譜儀分析。色譜柱為Agilent DB-wax(30 m ×0.53 mm,1.0μm);分彆使用氫火燄離子化檢測器(flame ionization detector,FID)和火燄光度檢測器(flame photometric detector,FPD)進行測定併對比結果。結果 FID測定乙烯砜和其水化產物的線性範圍分彆為0.5~20μg/mL 和2~100μg/mL;定量限分彆為2.6μg/mL和7.6μg/mL;檢測限分彆為0.8μg/mL和2.3μg/mL;加樣迴收率分彆為104.3%和92.4%。FPD測定結果與FID測定結果差異無統計學意義。結論使用FID已可以滿足檢驗需要,該方法靈敏、快速、專屬性彊,可用來同時控製產品中痕量的乙烯砜和其主要水化產物1,4-噻噁烷-1,1-二氧。
목적:건입교련파리산납주사액중교련제을희풍화기수화산물1,4-새악완-1,1-이양잔류량적측정방법。방법용을순췌취양품,을희풍화기수화산물용우을순,파리산납불용우을순생성백색침정,취상청액직접진양,용기상색보의분석。색보주위Agilent DB-wax(30 m ×0.53 mm,1.0μm);분별사용경화염리자화검측기(flame ionization detector,FID)화화염광도검측기(flame photometric detector,FPD)진행측정병대비결과。결과 FID측정을희풍화기수화산물적선성범위분별위0.5~20μg/mL 화2~100μg/mL;정량한분별위2.6μg/mL화7.6μg/mL;검측한분별위0.8μg/mL화2.3μg/mL;가양회수솔분별위104.3%화92.4%。FPD측정결과여FID측정결과차이무통계학의의。결론사용FID이가이만족검험수요,해방법령민、쾌속、전속성강,가용래동시공제산품중흔량적을희풍화기주요수화산물1,4-새악완-1,1-이양。
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.