摘要
用新型荧光试剂1，2-苯并-3，4-二氢咔唑-9-乙基氯甲酸酯作为柱前衍生化试剂，在乙腈中，以pH9的硼酸钠缓冲溶液为催化剂，40℃下衍生反应10min后获得稳定的荧光产物。在EclipseXDB-C8色谱柱上，通过梯度洗脱对5种多胺进行了分离和在线质谱定性。激发波长（λex）和发射波长Q。）分别为333nm和390nm。采用大气压化学电离源（APCI）正离子模式，实现了人尿中游离多胺的质谱定性及荧光定量测定。检出限（3S／N）在4．98～9．31fmol。此方法应用于尿样中多胺的测定，并测得回收率在949，6～989，6之间。
A new fluorescence reagent, 1,2-benzo-3, 4-dihydrocarbazole-9-ethyl chloroformate was used as pre-column derivatizing agent in an acetonitrile solution, catalyzed by the borate buffer of pH 9 to react with polyamines at 40 ℃ for 10 rain, to give stable fluorescence products. Five polyamines were then separated on the Eclipse XDB-C8 chromatographic column by gradient elution with acetonitrile-HzO solution of different concentrations, and on-line analyzed qualitatively with APCI mode by MS and quantitatively by HPLC with fluorescence detection at the wavelengths of （λex） 333 nm and （λem） 390 nm. Detection limits of the 5 polyamines （3S/N） found were in the range of 4. 98--9. 31 fmol. Test for recovery was made by addition of standard polyamine solutions to a urine sample, and the values of recovery found were in the range of 94%--98%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2009年第3期278-280,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
