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目的:建立衍生化后高效液相色谱法间接测定卤乙烯镁试剂中卤乙烯镁含量的方法。方法:通过卤乙烯镁和9-蒽甲醛的衍生反应合成9-蒽丙烯醇,采用高相液相色谱法测定9-蒽丙烯醇的含量。色谱柱为Agilent Zorbax SB-Pheny(250 mm×4.6 mm,5μm),流动相为乙腈∶0.1%磷酸(50∶50),流速1.5 mL/min,检测波长227 nm,柱温25℃,进样量15μL,采集时间20 min,以二苯甲酮作为内标物。根据衍生反应化学方程式计算卤乙烯镁的含量。结果:9-蒽丙烯醇在3.021~495.100μg/mL浓度范围内与峰面积有良好的线性关系,根据衍生反应化学方程式计算卤乙烯镁的含量,其结果(1.42 mol/L)与供应商报告结果一致。结论:对于卤乙烯镁试剂尤其是长期放置的卤乙烯镁试剂,采用衍生法和高效液相色谱法间接测定卤乙烯镁的含量,能消除烷基、炔烃的干扰,比常规直接滴定法更加准确、可行。
OBJECTIVE: To establish a method for the indirect determination of the content of vinyl halide magnesium in halogenated vinyl magnesium by derivatization high performance liquid chromatography. Methods: The 9-anthracene-propylene alcohol was synthesized by derivatization of vinyl halides with 9-anthracene-formaldehyde. The content of 9-anthracene-propylene alcohol was determined by high-performance liquid chromatography. The column was Agilent Zorbax SB-Pheny (250 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile: 0.1% phosphoric acid (50:50) at a flow rate of 1.5 mL / min and a detection wavelength of 227 nm at a column temperature of 25 ° C Amount of 15μL, collection time 20 min, benzophenone as an internal standard. Calculate the content of vinyl halide magnesium according to the derivatization reaction equation. Results: There was a good linear relationship between 9-anthracene-propylene alcohol and peak area in the concentration range of 3.021-495.100μg / mL. The content of vinyl halide was calculated according to the derivatization reaction equation. The result (1.42 mol / L) The result is the same. CONCLUSIONS: For the halogenated vinyl magnesium reagent, especially the long-lived halogenated vinyl magnesium reagent, the derivatization and high performance liquid chromatography are used to indirectly determine the content of vinyl halide magnesium, which can eliminate the interference of alkyl and alkyne more than conventional direct titration Accurate and feasible