摘要
合成了一种用于醇类分析的高灵敏度的荧光衍生化试剂2(4羧基苯基)4,5萘并咪唑(CNI),将其在二氯甲烷中于80℃条件下与醇缩合成酯,并采用RPHPLC法进行分离检测,色谱柱为ZorbaxBpC8柱(250mm×4.6mmi.d.),流动相为V(乙腈)∶V(甲醇)=90∶10的溶液,荧光检测波长λex345nm,λem485nm。同时,测定了人血清中的胆固醇,其最低检出质量浓度为1.0μgL。
A new sensitive pre column fluorescent derivatization method,which employs high performance liquid chromatography(HPLC) with fluorometric detection, for the determination of alcohols is described. The alcohols were transformed into the corresponding fluorescent esters by treating with 2 (4 carboxyphenyl) naphthoimidazole in dichloromethane in the presence of 4 piperidinopyridine (PIP) and 1 isopropyl 3 (3 dimethylaminopropyl) 1 carbodiimide perchlorate(IDC) at 80 ℃ for 10 min. The resultant mixture was analyzed by HPLC on a reversed phase column(Zorbax Bp C 8,4.6 mm i.d.×250 mm, 5 μm) with acetonitrile methanol (volume ratio was 90∶10) as mobile phase, and the sample volume was 20 μL. Monitored excitation and emission wavelengths were 345 nm and 485 nm respectively in determination of the alcohol. The calibration curve of cholesterol is linear between 0 and 2.5 g/L with correlation coefficient of 0.999 2. The average recovery was 96.15% with RSD of 1.39%. The lowest detectable mass concentration of cholesterol was 1.0 μg/L( S/N =3).
出处
《色谱》
CAS
CSCD
北大核心
2000年第1期10-13,共4页
Chinese Journal of Chromatography
关键词
高效液相色谱法
萘并咪唑
醇类测定
fluorescence derivatization
high performance liquid chromatography
2 (4 carboxyphenyl) naphthoimidazole
alcohols determination
