中南民族大学学报(自然科学版)
中南民族大學學報(自然科學版)
중남민족대학학보(자연과학판)
JOURNAL OF SOUTH-CENTRAL UNIVERSITY FOR NATIONALITIES(NATURAL SCIENCE EDITION)
2013年
2期
5-8
,共4页
沈静茹%王伟%余学红%蔡薇%张祎%刘武林
瀋靜茹%王偉%餘學紅%蔡薇%張祎%劉武林
침정여%왕위%여학홍%채미%장의%류무림
双[-6-氧-(3-脱氧柠檬酸单酯-4)]-β-环糊精%头孢氨苄%手性分离
雙[-6-氧-(3-脫氧檸檬痠單酯-4)]-β-環糊精%頭孢氨芐%手性分離
쌍[-6-양-(3-탈양저몽산단지-4)]-β-배호정%두포안변%수성분리
bis-[6-oxygen-(3-deoxycitric acid monoester-4)]-β-CD%cephalexin%chiral separation
用双[-6-氧-(3-脱氧柠檬酸单酯-4)]-β-环糊精为手性流动相添加剂,以有机弱酸的形式和三乙胺组成缓冲体系,在高效液相色谱(HPLC)中实现了头孢氨苄对映体的手性拆分.结合碳18硅胶键合(ODS-BP)柱为固定相,该缓冲液与不同比例乙腈混合形成流动相,考察了流动相配比、pH值、手性流动相添加剂浓度等因素对头孢氨苄2对对映体手性分离的影响.结果表明:在pH 8.8,流速0.6 mL/min,检测波长310 nm,添加剂浓度为5.0 mmol/L缓冲液的最佳条件下,可实现头孢氨苄4个对映异构体色谱峰的基线分离,最佳条件下4峰中相邻两峰分离度Rs 分别为3.41、5.34和8.93.
用雙[-6-氧-(3-脫氧檸檬痠單酯-4)]-β-環糊精為手性流動相添加劑,以有機弱痠的形式和三乙胺組成緩遲體繫,在高效液相色譜(HPLC)中實現瞭頭孢氨芐對映體的手性拆分.結閤碳18硅膠鍵閤(ODS-BP)柱為固定相,該緩遲液與不同比例乙腈混閤形成流動相,攷察瞭流動相配比、pH值、手性流動相添加劑濃度等因素對頭孢氨芐2對對映體手性分離的影響.結果錶明:在pH 8.8,流速0.6 mL/min,檢測波長310 nm,添加劑濃度為5.0 mmol/L緩遲液的最佳條件下,可實現頭孢氨芐4箇對映異構體色譜峰的基線分離,最佳條件下4峰中相鄰兩峰分離度Rs 分彆為3.41、5.34和8.93.
용쌍[-6-양-(3-탈양저몽산단지-4)]-β-배호정위수성류동상첨가제,이유궤약산적형식화삼을알조성완충체계,재고효액상색보(HPLC)중실현료두포안변대영체적수성탁분.결합탄18규효건합(ODS-BP)주위고정상,해완충액여불동비례을정혼합형성류동상,고찰료류동상배비、pH치、수성류동상첨가제농도등인소대두포안변2대대영체수성분리적영향.결과표명:재pH 8.8,류속0.6 mL/min,검측파장310 nm,첨가제농도위5.0 mmol/L완충액적최가조건하,가실현두포안변4개대영이구체색보봉적기선분리,최가조건하4봉중상린량봉분리도Rs 분별위3.41、5.34화8.93.
Using bis-[6-oxygen-(3-deoxycitric acid monoester-4)]-β-cyclodextrin as the chiral HPLC mobile phase additive, an organic weak acid(β-cyclodextrin derivative) and triethylamine as buffer system, enantioseparation of cefalexin enantiomers was achieved. Based on an ODS-BP column stationary phase and a mixed mobile phase of acetonitrile and the additive-triethylamine buffer, the effects of the ratio of mobile phase, pH value and the concentration of the chiral additive concentration on the separation of cephalexin 2 enantiomers were discussed. The results showed that under the optimum conditions:pH8. 8, 0. 6mL/min flow rate, ultraviolet detection wavelength of 310 nm, additive concentration of 5. 0 mmol/L, baseline separation of 4 peaks of cefalexin enantiomers could be obtained, with the Rs of adjacent peaks being 3. 41, 5. 34 and 8. 93,respectively.