抽象的

Determination of semicarbazide in marine crustaceans by ultra-performance liquid chromatography tandem mass spectrometry with an improved pre-treatment method

Jian Wang, Xiaojun Zhang, Shuai Zhang, Zhongyong Yan

An improved liquid chromatography-mass spectrometry method was developed for the determination of SEM in the marine crustaceans. First, the optimization of amount of hydrochloric acid added was made to ensure complete reaction in the SEM derivatization system. Secondly, five adsorbents (PSA, C18, Florisil, Al2O3 and MWCNT) were compared for the purifying effect of impurities in detecting SEM, the most suitable adsorbent was PSA. This method performed additional PSA clean-up procedure gives good linear range and met the FDA guide on Analytical Procedures and Methods Validation in LOD, LOQ and mean recovery. The chromatogram of spiked samples also showed less endogenous interference and gave clearer effect. Finally, by using this improved LC-MS/MS method, 12 different marine crustaceans were analyzed. Distribution of SEM in tissues was found from testing muscle, viscera, whole body and shell of each crustacean. SEM in different tissues showed the lowest SEM content distribution in muscle and highest SEM content in shells. It can be inferred that SEM, as an endogenous substance commonly found in marine crustaceans, come from shells