盐酸托莫西汀旋光异构体的手性拆分研究

目的:建立盐酸托莫西汀旋光异构体的手性拆分方法。方法:Waters 高效液相色谱仪,Chiralcel OD(250 mm×4.6 mm,5μm)手性柱,正己烷-异丙醇-二乙胺(80:20:0.2)为流动相,流速为1.0 mL·min~(-1),紫外检测波长为271 nm。结果:左旋盐酸托莫西汀峰和右旋盐酸托莫西汀峰能很好地分开,分离度为5.5,拖尾因子小于1.2,理论塔板数大于5000,该方法可以用来测定盐酸托莫西汀中的右旋异构体,最低检出限为4 ng。供试品右旋盐酸托莫西汀溶液在4 h 内基本稳定(RSD=2.4%),3批样品中右旋盐酸托莫西汀含量均低于0.5%。结论:本方法快捷、简便,灵敏度高,可以用于原料药中右旋盐酸托莫西汀含量的测定,结果满意。     

Synthesis,self‐association and chiroselectivity of isotopically labeled trianglamine macrocycles in the ion trap mass spectrometer

The synthesis and self‐association of chiral isotopically labeled trianglamine macrocycles under electrospray mass spectrometer conditions in an ion trap are described. A moderate diastereoselectivity in the self‐association process was observed providing a synthetic model system for the investigation of chiral self‐association in the gas phase. The first non‐covalently bound dimer exclusively bonded through aromatic–aromatic interactions was observed in the gas phase. Evidence for self‐association in solution was observed by diffusion nuclear magnetic resonance spectroscopy. Copyright © 2007 John Wiley & Sons, Ltd.     

以盐酸去甲万古霉素为手性选择剂毛细管电泳法分离西替利嗪对映体

目的:建立以阳离子表面活性剂碘化四丁基铵为电渗流改性剂,以盐酸去甲万古霉素为手性选择剂的毛细管电泳法分离西替利嗪对映体。方法:考察了盐酸去甲万古霉素浓度、Tris 浓度和缓冲液 pH 对分离的影响,对分离条件进行了优化。结果:在含0.04 g·L~(-1)碘化四丁基铵和1.0 mmol·L~(-1)盐酸去甲万古霉素的25 mmol·L~(-1)Tris 磷酸缓冲液(pH 4.5)的运行电解质体系中,西替利嗪对映体在分离电压为20 kV 的条件下得到良好分离,西替利嗪对映体分离度达1.8。结论:本法可用于西替利嗪对映体的分离。     

毛细管电泳和高效液相作氨氯地平异构体分离分析研究

目的：毛细管电泳和高效液相作氨氯地平异构体分离分析研究。方法：毛细管电泳采用未涂渍熔融石英毛细管75μm×68cm(有效长度50cm)；优化选择浓度为100mmol/L的Tris缓冲液,含有1．0%羟丙基-β-CD(用磷酸调节pH至3．0)；分离电压18kV；温度15℃。高效液相色谱柱为ULTRON ES-OVM手性柱,流动相：乙腈-0．02mol/L磷酸二氢钠溶液(pH 7．0)(20∶80)；流速1．0ml/min。结果：氨氯地平对映异构体分离良好。结论：该方法简单可靠、专属性强。     

左舒必利的毛细管电泳手性分离与纯度检查

目的:建立手性分离方法并检查左舒必利光学纯度。方法:通过手性拆分剂的种类及浓度、缓冲液的pH及浓度、温度及电压的优化,选择最佳的手性分离条件。结果:最佳分离条件缓冲液为100 mmol·L~(-1)磷酸盐缓冲液(用磷酸调pH4．0,内含18 mmol·L~(-1)β-环糊精硫酸钠盐);检测波长为254 nm;电压为15 kV;温度为22℃,基线分离了舒必利2个对映体。结论:建立的毛细管电泳法可用于左舒必利的质量控制和稳定性研究。     

手性药物代谢的立体选择性

手性药物的代谢具有多种立体选择性，且相互关联，共同影响药物的体内过程，也必将影响到药效和毒副作用。充分了解手性异构体的代谢过程有助于准确评价手性异构体的药理活性，并为临床合理用药提供依据。本文综述了手性药物代谢的各种立体选择性及其对代谢的影响。     

热聚合法制备二苯甲酰-L-酒石酸手性分子印迹聚合物I．热聚合条件的优化

以二苯甲酰-L-酒石酸(L-DBTA)为模板分子,甲基丙烯酸甲酯(MMA)等为功能单体,乙二醇二甲基丙烯酸酯(GDMA)为交联剂,采用热聚合方法合成了L-DBTA手性分子印迹聚合物(ML-DBTA),讨论了不同功能单体、功能单体的用量、交联剂的用量、聚合温度、聚合时间、溶剂等对ML-DBTA合成的影响.通过ML-DBTA对底物的结合实验和高效液相色谱分析,合成的ML-DBTA对模板分子L-DBTA具有很好的识别性,对L-DBTA的选择性比二苯甲酰-D-酒石酸(D-DBTA)高,其分离因子(α)可达2.79.优化的热聚合条件为n(L-DBTA)n(MMA)n(GDMA)=1420,聚合温度60℃,聚合时间48 h,溶剂为乙腈.     

金鸡纳生物碱在手性分离中的应用

综述了金鸡纳生物碱作为手性选择剂在高效液相色谱和毛细管电泳中分离光学异构体的应用。     

Biosynthesis of 12(S)-hydroxyeicosatetraenoic acid by bovine corneal epithelium

Microsomes of bovine corneal epithelium metabolized [¹⁴C]arachidonic acid extensively to [¹⁴C]12-hydroxyeicosatetraenoic acid. The biosynthesis was not stimulated by exogenous NADPH and it could be inhibited by over 90% with two lipoxygenase inhibitors, esculetin and eicosatetraynoic acid. Chiral phase high performance liquid chromatography showed that 12-HETE consisted of the 125 enantiomer. The results indicate biosynthesis by 12S-lipoxygenase of bovine corneal epithelium rather than by cytochrome P450.     

Resolution of the stereoisomers of baclofen by high performance liquid chromatography

The GABA analogue baclofen [3-(p-chlorophenyl)-4-aminobutanoic acid] has stereospecific actions on the peripheral and central nervous systems. This paper describes the resolution of tritium-labelled baclofen by high performance liquid chromatography on a reverse-phase C18 column using a chiral mobile phase. The method, which may have general application to certain other GABA analogues, affords optically pure (+)- and (-)-baclofen labelled with tritium to high specific activity suitable for ligand binding and other neurochemical studies.