色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
6期
612-615
,共4页
张虎%沈芒芒%童胜强%颜继忠
張虎%瀋芒芒%童勝彊%顏繼忠
장호%침망망%동성강%안계충
高效液相色谱%手性流动相添加法%阿卓乳酸%对映体拆分%磺丁基醚-β-环糊精
高效液相色譜%手性流動相添加法%阿卓乳痠%對映體拆分%磺丁基醚-β-環糊精
고효액상색보%수성류동상첨가법%아탁유산%대영체탁분%광정기미-β-배호정
high performance liquid chromatography( HPLC)%chiral mobile phase addition%atrolactic acid%enantioseparation%sulfobutyl ether-β-cyclodextrin(SBE-β-CD)
采用 C18反相色谱柱，以磺丁基醚-β-环糊精（SBE-β-CD）作为手性流动相添加剂，建立了阿卓乳酸对映体的高效液相色谱拆分方法。考察了环糊精衍生物类型、手性添加剂浓度、流动相 pH、流速和柱温对手性分离的影响，同时探讨了高效液相色谱采用磺丁基醚-β-环糊精分离阿卓乳酸对映体的分离机制及包结常数，确定了色谱条件为YMC-Pack ODS-A C18色谱柱（250 mm×4.6 mm，5μm），流动相为含25 mmol / L SBE-β-CD 的0.1 mol / L 磷酸盐缓冲液（pH 2.68）-乙腈（90∶10，v / v），流速为0.6 mL / min，柱温为30℃，紫外检测波长为220 nm。对映体的保留时间分别为26.65和28.28 min，分离度为1.68。本方法分离度好，简便易行，且比使用手性固定相分离更加经济。
採用 C18反相色譜柱，以磺丁基醚-β-環糊精（SBE-β-CD）作為手性流動相添加劑，建立瞭阿卓乳痠對映體的高效液相色譜拆分方法。攷察瞭環糊精衍生物類型、手性添加劑濃度、流動相 pH、流速和柱溫對手性分離的影響，同時探討瞭高效液相色譜採用磺丁基醚-β-環糊精分離阿卓乳痠對映體的分離機製及包結常數，確定瞭色譜條件為YMC-Pack ODS-A C18色譜柱（250 mm×4.6 mm，5μm），流動相為含25 mmol / L SBE-β-CD 的0.1 mol / L 燐痠鹽緩遲液（pH 2.68）-乙腈（90∶10，v / v），流速為0.6 mL / min，柱溫為30℃，紫外檢測波長為220 nm。對映體的保留時間分彆為26.65和28.28 min，分離度為1.68。本方法分離度好，簡便易行，且比使用手性固定相分離更加經濟。
채용 C18반상색보주，이광정기미-β-배호정（SBE-β-CD）작위수성류동상첨가제，건립료아탁유산대영체적고효액상색보탁분방법。고찰료배호정연생물류형、수성첨가제농도、류동상 pH、류속화주온대수성분리적영향，동시탐토료고효액상색보채용광정기미-β-배호정분리아탁유산대영체적분리궤제급포결상수，학정료색보조건위YMC-Pack ODS-A C18색보주（250 mm×4.6 mm，5μm），류동상위함25 mmol / L SBE-β-CD 적0.1 mol / L 린산염완충액（pH 2.68）-을정（90∶10，v / v），류속위0.6 mL / min，주온위30℃，자외검측파장위220 nm。대영체적보류시간분별위26.65화28.28 min，분리도위1.68。본방법분리도호，간편역행，차비사용수성고정상분리경가경제。
A method was established for the enantioseparation of atrolactic acids using high performance liquid chromatography with sulfobutyl ether-β-cyclodextrin( SBE-β-CD ) as the chiral mobile phase additive,and a C18 reversed-phase column. The influences of the different types of cyclodextrin derivatives,the concentration of chiral mobile phase additive,pH value of the mobile phase,the flow rate and column temperature on the peak resolution were investiga-ted. The separation mechanism for atrolactic acids by high performance liquid chromatography using chiral mobile phase additive,as well as the formation of inclusion complex between SBE-β-CD and atrolactic acid was studied. In addition,the formation constant was calculated. The enantioseparation was carried out on a reversed-phase column YMC-Pack ODS-A C 18(250 mm× 4. 6 mm,5 μm)with chiral mobile phase consisted of 0.1 mol/L phosphate buffer at pH 2.68 containing 25 mmol/L SBE-β-CD-acetonitrile(90∶10,v/v). The detection wavelength was 220 nm. The flow rate was 0.6 mL/min and the column temperature was 30℃.The retention times of atrolactic acids were 26.65 and 28.28 min,and the peak resolution of 1.68 was achieved. The above established method proves to be a simple and economical way for analytical enanti-oseparation of atrolactic acid with high peak resolution.
