CAJ | 학술논문

目的建立一种顶空进样气相色谱法,以定量检测硫酸庆大霉素中甲醇的残留量. 方法使用DB-624气相色谱柱,尺寸为20 m(长)×0.53 mm(内径)×3.00 μm(膜厚).以氮气为载气,流经气化室与气化的甲醇和乙醇混合,然后混合气体进入色谱柱进行分离.甲醇和乙醇气体先后进入氢火焰离子化检测器,在氢火焰作用下化学电离形成离子流,可通过测定离子流强度对其进行检测.结果甲醇气体与乙醇气体完全分离,在考察范围内有良好的线性,相关系数为0.999 28.甲醇最低检测限为0.40μg/ml,定量限为1.32 μg/ml.甲醇平均回收率为99.99％.两名分析员分别对同一浓度级6个平行测试液检测,测定结果的相对标准偏差为2.7％.结论建立的方法灵敏度和准确度均达到有机溶剂残留量的检测要求,可用于硫酸庆大霉素中甲醇残留量的定量检测.
목적 건립일충정공진양기상색보법,이정량검측류산경대매소중갑순적잔류량. 방법 사용DB-624기상색보주,척촌위20 m(장)×0.53 mm(내경)×3.00 μm(막후).이담기위재기,류경기화실여기화적갑순화을순혼합,연후혼합기체진입색보주진행분리.갑순화을순기체선후진입경화염리자화검측기,재경화염작용하화학전리형성리자류,가통과측정리자류강도대기진행검측.결과 갑순기체여을순기체완전분리,재고찰범위내유량호적선성,상관계수위0.999 28.갑순최저검측한위0.40μg/ml,정량한위1.32 μg/ml.갑순평균회수솔위99.99％.량명분석원분별대동일농도급6개평행측시액검측,측정결과적상대표준편차위2.7％.결론 건립적방법령민도화준학도균체도유궤용제잔류량적검측요구,가용우류산경대매소중갑순잔류량적정량검측.
Objective To establish a head-space gas chromatography for quantifying residual methanol in gentamycin sulfate.Methods DB-624 chromatographic column (20 m × 0.53 mm × 3.00μm)and nitrogen (as a carrier gas) were used.The nitrogen was mixed with gasification methanol and ethanol in a gasification chamber.Then,the mixed gas entered the chromatographic column to be separated.Methanol and ethanol gases entered a hydrogen flame ionization detector successively and formed ion current under action of hydrogen flame.They were tested by measurement of intensity of ion current.Results Methanol and ethanol gases were completely separated.A good linearity was observed within the scope of investigation and the correlation coefficient was 0.999 28.The detection and quantification limits of methanol were 0.40 and 1.32 μg/ml,respectively.The average recovery was 99.99％.Six parallels were prepared from methanol solutions of same concentration magnitude and determined independently by two analysts.The relative standard deviation of the results was 2.7％.Conclusions The sensitivity and accuracy of the established method meet the detection requirements of organic solvent residuex The method can be used for quantification of residual methanol in gentamycin sulfate.