LC/ES-MS存PTS国际实验室间比较测试中的应用

本文应用LC／ES－MS分析了水样品W1和W2、土样S和萃取液样品E中有毒化学品及其前体或降解产物，并初步探讨了这些化合物的断裂机理。

Identification,synthesis and characterization of an unknown process related impurity in eslicarbazepine acetate active pharmaceutical ingredient by LC/ESI-IT/MS,~1H,^(13)C and ~1H-~1H COSY NMR

A new impurity was detected during high performance liquid chromatographic （HPLC） analysis of eslicarbazepine acetate active pharmaceutical ingredient. The structure of unknown impurity was postulated based on liquid chromatography mass spectrometry using electrospray ionization and ion trap analyzer （LC/ESI-IT/MS） analysis. Proposed structure of impurity was unambiguously confirmed by synthesis followed by characterization using 1H, 13C nuclear magnetic resonance spectrometry （NMR）, 1H-1H correlation spectro-scopy （COSY） and infrared spectroscopy （IR）. Based on the spectroscopic and spectrometric data, unknown impurity was characterized as 5-carbamoyl-10,11-dihydro-5H-dibenzo[b,f]azepin-10-yl propionate.

BTTN与NG混合物的电喷雾电离质谱研究

利用大气压电喷雾电离 液相色谱 质谱联用(API ESI LC MS)技术分离和检测丁三醇三硝酸酯(BTTN)和丙三醇三硝酸酯(NG)的二元混合物,BTTN和NG的分离用反相高效液相色谱在C18柱上进行,在225nm处实施。乙醇 水(1 1,V/V)混合液为流动相,流速为0.2ml·min-1.研究了CapEx电压、pH值的变化、反吹气温度、电离方式对BTTN和NG质谱的影响。结果表明,用负离子方式检测,CapEx电压、pH值分别为-100V和7,反吹气温度为100℃时可得到较理想的质谱图。