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目的:建立了毛细管气相色谱法测定啤酒花颗粒中17种有机磷的分析方法。方法:本方法采用乙腈加磷酸缓冲溶液提取,过C18炭黑复合柱净化、NH2炭黑复合柱净化、氟罗里硅土柱净化,来消除基质影响,采用HP50+毛细管柱和火焰光度检测器测定,外标法定量,配制两种不同的校准曲线,溶剂标准曲线(SC)和啤酒花基质标准曲线(MC)。用两种不同的校准曲线对同一采集的数据计算线性范围、相关系数、线性方程、检出限、回收率及相对标准偏差。结果:乙腈加磷酸缓冲溶液提取,过C18炭黑复合柱净化、NH2炭黑复合柱净化,能够降低基质增强效应,回收率符合2002/657/EG中70%～110%的规定。结论:实验结果表明,该方法简便、快速、准确,各项技术指标均满足农药残留检测的要求,适合啤酒花颗粒等复杂基质中有机磷含量的测定。
OBJECTIVE: To establish a method for the determination of 17 organophosphorus in hops by capillary gas chromatography. Methods: The method was extracted with acetonitrile and phosphoric acid buffer solution, purified with C18 carbon black composite column, purified with NH2 carbon black composite column and purified with Florisil silica column to eliminate the influence of matrix. HP50 + capillary column and flame photometric detector , External standard method to quantify, prepare two different calibration curves, solvent standard curve (SC) and hops matrix curve (MC). Two different calibration curves were used to calculate the linear range, correlation coefficient, linear equation, detection limit, recovery rate and relative standard deviation for the same collected data. Results: Acetonitrile was extracted with phosphate buffer solution, purified with C18 carbon black composite column and purified with NH2 carbon black composite column. The matrix enhancement effect could be reduced and the recovery rate accorded with 70% ~ 110% of 2002/657 / EG. Conclusion: The experimental results show that the method is simple, rapid and accurate, and all the technical indexes meet the requirements of pesticide residue detection. It is suitable for the determination of organic phosphorus content in complex matrix such as hops particles.