Organoaluminum compounds have been employed as catalysts in many reactions. However, due to their high reactivity of the Al−C bond towards water or air, the accurate analysis and detection of organoaluminum compounds are still challenging. Here we demonstrate the possibility of rapidly and precisely detecting the purity and impurities of triethylaluminium (TEAL). An indirect GC-MS method via alcoholysis reaction using a designed alcoholysis reactor was adopted to detect and separate the main components and impurities of the synthesized TEAL. Previously, the nuclear magnetic resonance (NMR) and the inductively coupled plasma-mass spectrometer (ICP-MS) methods were also selected to detect the main compounds in the synthesized TEAL. The impurities in TEAL was identified as n-butyl aluminum, and the purity of synthesized TEAL is 97.47 % with high accuracy (ca. 99 %). This work suggests a new strategy to detect the purity and impurities of some kind of hazardous compounds.
Zhou Lizi,Yang Zhaoguang,Zhi Tiantian,Zhou Zhou,Wang Xiaochen,Ren Chunmei,Qiu Bo
Succinylacetone was known to be a toxic metabolite of tyrosine in human and animals caused by blockage of the final step in tyrosine degradation pathway, but its existence in plant was unclear though the metabolic disturbance of tyrosine was also found in plant. A GC-MS method for determination of succinylacetone in Arabidopsis thaliana was developed for the first time. Both oximation and silylation were applied in the derivation procedure, and a low-temperature condition before completion of oximation was found to be necessary to obtain good linearity of the calibration curve due to the thermolability of succinylacetone. The specific chromatogram pattern formed by the four isomers of succinylacetone derivatives provided a helpful feature for its identification. The detection limit of the proposed method was 0.25 ppm in A. thaliana . The recoveries were between 95.4 and 109.3 % with the coefficient of variation ranging from 4.36 to 7.81 % for intra-day assays and 6.47 to 8.52 % for inter-day assays. Application to wild-type and the short-day sensitive cell death 1 mutant of A. thaliana represented an obvious correlation between the measured amount of succinylacetone and wilting symptom, suggesting the proposed method could be a powerful tool in further study on toxicology of succinylacetone and tyrosine catabolism in plants.
危险品化学品经营许可证（带存储）