Zhao Yuan-Yuan, Cai Ling-Shuang, Jing Zhi-Zhong, Wang Hong, Yu Jian-Xin, Zhang Hua-Shan
College of Chemistry and Molecular Science, Wuhan University, Wuhan 430072, China.
J Chromatogr A. 2003 Dec 22;1021(1-2):175-81. doi: 10.1016/j.chroma.2003.09.025.
A simple, selective and sensitive approach was developed for the quantitation of aliphatic amines in lake water applying a new reagent (N-succinimidyl benzoate, SIBA), synthesized in the laboratory of the authors. Derivatization of the n-C1-C6 aliphatic monoamines and dimethylamine in aqueous solution with SIBA was followed by headspace solid-phase microextraction (SPME). Derivatives were identified by gas chromatography-mass spectrometry and determined by gas chromatography-flame ionization detection. Both derivatization and SPME conditions have been optimized. Derivatizations were performed in borate buffer (pH 8.8), at 60 degrees C for 22 min. SPME was carried out from saturated sodium chloride solution, at 80 degrees C for 60 min, desorption at 250 degrees C for 2 min. Detection limit of derivatized amines proved to be 0.13-7.2 nmol/l, while recovery of amines from lake water samples, in the concentration range of 100-200 microg/l, varied from 94.1 to 102.7%.
利用作者实验室合成的一种新型试剂（N - 琥珀酰亚胺基苯甲酸酯，SIBA），开发了一种简单、选择性好且灵敏的方法，用于定量湖水中的脂肪胺。用SIBA对水溶液中的正C1 - C6脂肪族单胺和二甲胺进行衍生化，然后进行顶空固相微萃取（SPME）。衍生物通过气相色谱 - 质谱联用仪进行鉴定，并用气相色谱 - 火焰离子化检测器进行测定。衍生化和SPME条件均已优化。衍生化在硼酸盐缓冲液（pH 8.8）中于60℃进行22分钟。SPME在饱和氯化钠溶液中于80℃进行60分钟，在250℃解吸2分钟。衍生化胺的检测限为0.13 - 7.2 nmol/L，而湖水中胺类在100 - 200 μg/L浓度范围内的回收率为94.1%至102.7%。
