牙本质中天冬氨酸消旋化程度的测定——手性毛细管气相色谱法与高效液相色谱法的比较  

Determination of Degree of Racemization of Aspartic Acid in Dentine Comparison of Chiral Capillary Gas Chromatography with High Performance Liquid Chromatography

作　　者：段盛慧[1] 张晓朋 谢妮[1] 范垂昌[2,3] 刘俊亭[2,3] 傅世江 

机构地区：[1]中国医科大学预防医学系 [2]中国医科大学法医系 [3]中国医科大学呼吸病研究所

出　　处：《色谱》1996年第6期484-486,共3页Chinese Journal of Chromatography

摘　　要：应用手性毛细管气相色谱法（酸性异丙醇、三氟乙酸酐为衍生试剂）、高效液相色谱法（邻苯二甲醛－Ｎ－乙酰－Ｌ－半胱氨酸为手性衍生试剂）同时测定人类第一磨牙牙本质中天冬氨酸的消旋化程度，结果表明，两者均可有效地用于天冬氨酸对映体的分离测定，但气相色谱检测限（０．２ｐｍｏｌ）低于高效液相色谱（１．０ｐｍｏｌ），而变异系数（７％）、总分析时间（１００ｍｉｎ）均高于高效液相色谱（分别对应为４％，３１ｍｉｎ）。Aspartic acid(Asp) enantiomers which were taken from human dentine were derivatized by acidic isopropanol and trifluoroacetic acid anhydride. The derivatives were analysed by capillary GC with chiral phase of cross linked polycyanoethyl vinylsilane L valine tert butylamine at column temperature of 127℃ and FID detector. The Asp enantiomers were also derivatized into fluorescence diastereomers by OPA NAC, prior to the determination by reversed phase HPLC with column of LiChrosorb RP 18, mobile phase of MeOH 8%+NaAc 92% (pH 5.7, 50 mmol/L)and fluorenscence monitor at λ ex =340nm and λ em = 445nm. Resolutions were 1.2 in GC and 1.45 in HPLC. Method with HPLC is simpler, and more rapid than that with GC, although its detectable limit (1pmol) is higher than that of GC(0.2pmol).

关 键 词：气相色谱 高效液相色谱 天冬氨酸 牙本质 消旋化 

分 类 号：Q593.9[生物学—生物化学]