You Jinmao, Zhao Huaixin, Sun Zhiwei, Xia Lian, Yan Tao, Suo Yourui, Li Yulin
Northwest Plateau Institute of Biology, Chinese Academy of Sciences, Xining, PR China.
J Sep Sci. 2009 May;32(9):1351-62. doi: 10.1002/jssc.200800724.
A simple, sensitive method for the determination of aliphatic amines based on a sulfonylation reaction using 10-ethyl-acridine-3-sulfonyl chloride (EASC) as pre-column labeling reagent with fluorescence detection and APCI-MS identification has been developed. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by HPLC with an excitation maximum at lambda(ex) 270 nm and an emission maximum at lambda(em) 430 nm. Identification of derivatives was carried out by online post-column MS in positive-ion mode. Comparing with the widely used 5-dimethylaminonaphthalene-1-sulfonylchloride (Dansyl-Cl), EASC-amine derivatives not only exhibited high fluorescence but also exhibited excellent MS ionizable potential. Detection limits obtained from 0.10 pmol injection, at a S/N of 3, were 4.0-12.7 fmol. The mean intra- and inter-assay precision for all aliphatic amine levels were <3.84 and 3.21%, respectively. Excellent linear responses were observed with coefficients of >0.9995.
开发了一种基于磺酰化反应的简单、灵敏的脂肪胺测定方法,该方法使用10-乙基吖啶-3-磺酰氯(EASC)作为柱前标记试剂,采用荧光检测和大气压化学电离质谱(APCI-MS)进行鉴定。标记的衍生物具有高稳定性,足以通过高效液相色谱(HPLC)进行有效分析,其激发波长最大值(λex)为270 nm,发射波长最大值(λem)为430 nm。衍生物的鉴定通过在线柱后质谱在正离子模式下进行。与广泛使用的5-二甲基氨基萘-1-磺酰氯(丹磺酰氯,Dansyl-Cl)相比,EASC-胺衍生物不仅具有高荧光性,而且具有出色的质谱电离潜力。在进样量为0.10 pmol、信噪比为3时获得的检测限为4.0 - 12.7 fmol。所有脂肪胺水平的平均批内和批间精密度分别<3.84%和3.21%。观察到良好的线性响应,相关系数>0.9995。