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某些反相高效液相色谱柱在分析碱性化合物时的亲水相互作用特性。

The hydrophilic interaction like properties of some reversed phase high performance liquid chromatography columns in the analysis of basic compounds.

机构信息

Strathclyde Institute of Pharmacy and Biomedical Sciences, 27 Taylor Street, Glasgow G40NR, United Kingdom.

出版信息

J Chromatogr A. 2011 Mar 18;1218(11):1486-91. doi: 10.1016/j.chroma.2011.01.036. Epub 2011 Jan 19.

Abstract

The hydrophilic interaction chromatography (HILIC) like properties of an ACE cyano (CN) HPLC column was studied for the separation of some basic compounds. Good separation of a test mix of basic compounds was obtained with a mobile phase consisting of acetonitrile/water (95:5) containing 3.25 mM ammonium acetate. The retention times of the basic compounds decreased with increased ionic strength or with increased water content in the mobile phase. When Trishydroxymethyl aminomethane (Tris) (pK(a) 8.0), which is a weaker amine than ammonia (pK(a) 9.3), was used as an additive in the mobile phase retention of the basic compounds was increased. The ACE CN column gave excellent peak shapes for all the basic compounds. The utility of the column for impurity profiling of two basic drugs was tested and some impurities in oxprenolol were characterised by interfacing with Fourier transform mass spectrometry. It was also observed that ACE butyl and ACE phenyl columns retained basic compounds when the columns were eluted with a mobile phase consisting of acetonitrile/water (95:5) containing 3.25 mM ammonium acetate.

摘要

亲水性相互作用色谱(HILIC)类似于 ACE 氰基(CN)HPLC 柱的性质,用于分离一些碱性化合物。用含有 3.25mM 乙酸铵的乙腈/水(95:5)作为流动相,可很好地分离碱性化合物的测试混合物。碱性化合物的保留时间随流动相中离子强度的增加或含水量的增加而降低。当三羟甲基氨基甲烷(Tris)(pK(a)8.0),比氨(pK(a)9.3)弱的胺作为流动相添加剂使用时,碱性化合物的保留时间增加。ACE CN 柱对所有碱性化合物都给出了极好的峰形。该柱用于两种碱性药物杂质剖析的实用性已得到检验,并通过与傅里叶变换质谱联用,对氧烯洛尔中的一些杂质进行了表征。还观察到,当用含有 3.25mM 乙酸铵的乙腈/水(95:5)作为流动相洗脱时,ACE 丁基和 ACE 苯基柱也保留碱性化合物。

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