摘要
采用反相高效液相色谱法测定了盐酸瑞芬太尼合成过程中两种中间体的含量,作为其生产过程的质量控制方法。采用KromasilC18(4.6mm×250mm,5μm)色谱柱,以乙腈-磷酸水溶液(pH3.0)(30∶70,v/v)为流动相,柱温为室温,UV检测波长240nm。两种中间体1-苄基-4-氰基-4-苯胺基哌啶(中间体I)与1-苄基-4-氨甲酰基-4-苯胺基哌啶(中间体II)达基线分离,其线性范围分别为0.03～6.6mg·L-1及0.06～6.6mg·L-1。在定量限以上的日内及日间重现性RSD≤1.0%,二者的平均回收率高于98.90%。本法简便、快速,结果准确,重现性好,可用于盐酸瑞芬太尼合成过程中两种中间体的质量控制。
Reversed phase liquid chromatography was applied to the determination of two intermediates during the synthetic process of remifentanil hydrochloride as a method of quality control.The Kromasil C18（4.6mm × 250mm,5μm） column was used with the mobile phase of acetonitrile-phosphoric acid in water （pH 3.0） （30： 70,v/v） at ambient temperature.The analytes were detected at UV 240nm.Under the optimum condition,the two intermediates,1-benzyl-4-nitrile-4-anilinopiperidine（ab.Intermediate I） and 1-benzyl-4-carbamoyl-4-anilinopiperidine （ab.Intermediate II） were baseline separated.The linear ranges of the two intermediates were 0.03 ～ 6.6 mg· L-1 and 0.06 ～ 6.6 mg· L-1,respectively.Recoveries of greater than 98.90% with intra-and inter-day precision（RSD） less than 1.0% were obtained for the two compounds at the concentrations above the LOQ.The method was simple,rapid and accurate,which can be applied in the quality control of the two intermediates during the synthesis of remifentanil.
出处
《广州化工》
CAS
2010年第8期186-188,共3页
GuangZhou Chemical Industry
基金
宜昌市科技发展计划项目(A06104)
