高效液相色谱法定量分析d,l-HMPAO及其冻干药盒

摘要: 采用反相高效液相色谱法，在国内外首次建立了鉴定ＨＭＰＡＯ（六甲基丙二胺肟）非对映异构体和ｄ，ｌ－ＨＭＰＡＯ（外消旋－六甲基丙二胺肟）冻干药盒的定量分析方法．研究出一种最佳的流动相分离分析ＨＭＰＡＯ非对映异构体的纯度和冻干药盒中ｄ，ｌＨＭＰＡＯ的含量。色谱参数：理论塔板高小于０．０６ｍｍ，总分离时间为５．５ｍｉｎ，分离度大于５。测得ｍｅｓｏ－ＨＭＰＡＯ和ｄ，ｌ－ＨＭＰＡＯ的紫外最小检出量各为１×１０￣（－８）ｇ和５×１０￣（－７）ｇ，精密度为５％，重加回收率在９４％－１０７％。实验表明，本方法具有准确、快速、稳定和简便等优点，适于常规质量控制，并已成功地用于本院合成的ＨＭＰＡＯ非对映异构体及其所生产的ｄ，ｌ－ＨＭＰＡＯ冻干药盒和对照品英国Ａｍｅｒｓｈａｍ公司同类制品的定量分析。

Abstract: THE QUANTITATIVE ANALYSIS OF d,l-HMPAO AND ITS FREEZE-DRIED KIT BY HPLCCHEN SUZHEN（China Institute of Atomic Energy，P.O. Box 275，Beijing，102413）ABSTRACT A quantitative analysis method of reversed phase high performance liqud chromatogra-phy （HPLC）is first established to study the stereoisomeric purity of HMPAO and d，l-HMPAO content of d，l-HMPAO freeze-dried kit．An optimized mobile phase has been se-lected to obtain chromatographic parameters which are better than those in all of referencesup to now. The theoretical plate height is less thari 0．06mm. The total time of separation isonly 5．5min when the flow rate is 1ml／min. The separation factor is larger than 5．The min-mum detecting weights of meso-HMPAO and d，l-HMPAO are 1×10~(-8)g and 5×10~(-7)g，re-spectively. The precision and the additional recovery of this method are 5％and 94％─107％，respectively． The method has the advantages of accuracy，rapidity，simplicity and suitabilityfor the routine work and has been successfully applied to analyze d，l-HMAPO in steroiso-mer and kit，which are made in China Instetute of Atomic Energy and Amersham Internation-al plc UK. Key words d，l-HMPAO Freeze-dried kit High performance liquid chromatography（HPLC）