Preparation Process Of LC-MS Grade Acetonitrile And Chemical Industry Standard Formulation

With the development of science and society, the demand of purity and applicability of chemical reagent is higher and higher in many high-tech fields. Such as chromatographic analysis, mass spectrometry, pesticide residue detection of fruits and vegetables and other food, biological pharmaceutical and organic synthesis are all need compatible organic solvents. Such as general chromatography grade, analytical grade reagent for laboratory research, pesticide residue grade reagent of food detection, LC-MS grade reagent of mass spectrometry detection. LC-MS grade acetonitrile is the most commonly used mass spectrum grade reagents, and have been widely used in chemical products test, food quality test, biological pharmacy test; LC-MS grade acetonitrile is common mobile phase solvents or reactants in modern high-precision analytical instruments such as liquid chromatography-mass spectrometry. Because of LC-MS grade acetonitrile products and standard are fall behind foreign products in domestic, this study focused on the purification process and standard specification of LC-MS grade acetonitrile. The main works are as follows:1. The purification process of LC-MS grade acetonitrile was studied, the industrial acetonitrile as crude after purification approaches including adsorption, oxidation and distillation. The experimental results show that the quality of acetonitrile product can comparable to foreign reagent index which can be suitable for mass spectrometry analysis. The optimized process parameters are:firstly utilizing100-200mesh of alumina as adsorbent, then utilizing potassium permanganate as oxidant, the amount of oxidant is1.25g/L, finally utilizing packed tower as distillation equipment, the temperature of the tower is86℃with reflux ratio of5:5, the yield is approximately75%. The product using this method has low level impurities content can meet the needs of mass spectrometry, and simple to operate, cost saving has broad market prospect.2. Chemical industry standard formulation work of LC-MS grade acetonitrile was carried out:through the method of combining the domestic and foreign market research and experiment, formulated the LC-MS grade acetonitrile standard that can suite China’s national conditions and meet market’s needs. Study whole detection methods system of LC-MS grade acetonitrile. Uses gas chromatography-mass spectrometer analysis and qualitative impurities in industrial grade acetonitrile, and use ultraviolet spectrophotometer and gas chromatograph, liquid mass spectrometer and inductively coupled plasma mass spectrometer test the acetonitrile product with the whole detection methods system of LC-MS grade acetonitrile, and in accordance with the LC-MS grade acetonitrile standard to evaluate the quality of the product, and comparison with the foreign products.