泉州师范学院学报
泉州師範學院學報
천주사범학원학보
JOURNAL OF QUANZHOU NORMAL COLLGEG
2014年
2期
36-39
,共4页
高效液相色谱法%天冬氨酸对映体%手性拆分
高效液相色譜法%天鼕氨痠對映體%手性拆分
고효액상색보법%천동안산대영체%수성탁분
high performance liquid chromatography (HPLC )%aspartic acid enantiomers%chiral resolution
用邻苯二甲醛(OPA)、N-乙酰-L-半胱氨酸为衍生试剂对天冬氨酸对映体进行柱前衍生.采用ZORBAX Eclipse AAA 4.6×150 mm,5μm 色谱柱,以0.05 mol/L pH 5.08的醋酸钠溶液与甲醇按57∶43体积比作为流动相,流速0.5 mL/min,柱温40℃下,考察高效液相色谱柱前衍生化法分离测定天冬氨酸对映体的效果.结果显示:在3.5 min 内分离出天冬氨酸对映体.在20~100 nmol/mL 线性范围内,线性关系良好,相关系数在0.99915以上,相对标准偏差在0.65%~1.70%之间.该法快速、简便、分离度高,能够完全分离DL-天冬氨酸对映体,并对其他氨基酸对映体的分离有良好的参考价值.
用鄰苯二甲醛(OPA)、N-乙酰-L-半胱氨痠為衍生試劑對天鼕氨痠對映體進行柱前衍生.採用ZORBAX Eclipse AAA 4.6×150 mm,5μm 色譜柱,以0.05 mol/L pH 5.08的醋痠鈉溶液與甲醇按57∶43體積比作為流動相,流速0.5 mL/min,柱溫40℃下,攷察高效液相色譜柱前衍生化法分離測定天鼕氨痠對映體的效果.結果顯示:在3.5 min 內分離齣天鼕氨痠對映體.在20~100 nmol/mL 線性範圍內,線性關繫良好,相關繫數在0.99915以上,相對標準偏差在0.65%~1.70%之間.該法快速、簡便、分離度高,能夠完全分離DL-天鼕氨痠對映體,併對其他氨基痠對映體的分離有良好的參攷價值.
용린분이갑철(OPA)、N-을선-L-반광안산위연생시제대천동안산대영체진행주전연생.채용ZORBAX Eclipse AAA 4.6×150 mm,5μm 색보주,이0.05 mol/L pH 5.08적작산납용액여갑순안57∶43체적비작위류동상,류속0.5 mL/min,주온40℃하,고찰고효액상색보주전연생화법분리측정천동안산대영체적효과.결과현시:재3.5 min 내분리출천동안산대영체.재20~100 nmol/mL 선성범위내,선성관계량호,상관계수재0.99915이상,상대표준편차재0.65%~1.70%지간.해법쾌속、간편、분리도고,능구완전분리DL-천동안산대영체,병대기타안기산대영체적분리유량호적삼고개치.
Aspartic acids enantiomers were precolumn derivatized with O-phthalaldehyde(OPA)and N-acetyl-L-cysteine through a ZORBAX Eclipse AAA column (4.6 ×150 mm,5 μm).The mobile phase was methanol-sodium acetate solution(adjusting to pH = 5.08)= 43 ∶ 57 (V/V ).The flow rate was 0.5 mL/min.The column temperature was 40 ℃.The influence of precolumn derivatization on the enantiomeric separations of Aspartic acids were investigated.The results were determined as follows. The separation was finished in 3.5minute.The calibration curve was linear in the range of 20 ~ 100 nmol/mL.The RSD were 0.65% ~ 1.70%.The analytical method was rapid,simple with high resolution and could be used as a reference of chiral resolution to other amino acid enantiomers .