摘要
皮质醇是临床医学和药物学研究中的重要测定指标,但皮质醇测定的量值溯源问题尚待解决。本工作对皮质醇纯品中杂质的定性定量以及纯度的测定进行了研究。采用HPLC-IT-TOF对与主成分结构类似的杂质进行定性分析,并采用HPLC-MS/MS对杂质含量进行定量测定。采用卡尔费休库仑法、顶空气相色谱法、电感耦合等离子体质谱法对其他杂质进行定量分析,用质量平衡法计算皮质醇纯品的纯度,结果为99.18%,扩展不确定度为U=0.18%(k=2),并用定量核磁法对测定结果进行了验证。结果表明,两种方法定值结果的一致性较好,说明所建立的定性及定量方法准确可靠,对激素类及其他有机纯物质的定性和定量有较好的指导作用。
Hydrocortisone is an important biomarker in clinical medicine and pharmacology, but the traceability of hydrocortisone hasn＇t been settled yet. Identification and quantification of impurities in hydrocortisone as well as purity of hydrocortisone were studied in this work. Structure analysis and identification of related structure impurities were carried out by HPLC-IT-TOF. Related structure impurities were quantified by HPLC-MS/MS. The methods of Karl Fischer Coulometric, headspace GC and ICP-MS were used for quantifica- tion of other impurities. Purity of hydrocortisone is concluded to be 99.18% by mass balance method with an expended uncertainty of U=0.08% （k=2）. The result was further confirmed by quantitative NMR spectroscopy method. The results of two methods are ingood agreement, which indicate that qualitative and quantitative analysis method established in this work is accurate and reliable. Moreover, this method has instructive significance to the qualitative and quantitative analysis of pure steroids and other pure organic substances.
出处
《质谱学报》
EI
CAS
CSCD
北大核心
2014年第5期413-419,共7页
Journal of Chinese Mass Spectrometry Society
基金
国家科技基础专项(2011FY130100)
国家科技支撑计划课题(2013BAK10B01)资助
关键词
皮质醇
杂质
定性
定量
纯度
hydrocortisone
impurities
identification
quantification
purity
