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应用高效液相色谱-三重四极杆质谱联用仪(HPLC-MS/MS)建立了粮谷中克瘟散的分析方法。实验确立以90%乙腈水溶液为提取溶剂,应用ProElut AFT-3固相萃取柱进行净化,乙腈-0.1%甲酸溶液(6+4,V/V)为定容液的预处理方法。实验结果表明,在最优条件下,目标物在1.0~100.0μg/L范围内线性良好,5种基质匹配(面粉、小米、糙米、玉米、大米)曲线的相关系数(r)均大于0.9997,加标实验回收率在78.5%~112.3%之间,相对标准偏差(RSD)为3.4%~13%,方法检出限(LOD,S/N≥3)为0.3μg/kg,定量限(LOQ,S/N≥10)为1.0μg/kg。经方法学验证,方法适用于粮谷中克瘟散的检测与定量测定。
A HPLC-MS / MS method was developed for the determination of g blast in grain. Experiments established 90% acetonitrile aqueous solution as the extraction solvent, using ProElut AFT-3 solid phase extraction column for purification, acetonitrile -0.1% formic acid solution (6 +4, V / V) as a pretreatment solution of constant volume. The experimental results showed that under the optimum conditions, the linearity of the target ranged from 1.0 to 100.0 μg / L. The correlation coefficients (r) of the five matrix matches (flour, millet, brown rice, corn and rice) The recoveries were in the range of 78.5% -112.3%. The relative standard deviations (RSDs) were 3.4% ~ 13%. The limits of detection (LOD, S / N≥3) were 0.3μg / , S / N ≧ 10) was 1.0 μg / kg. The methodological verification, the method is suitable for the detection and quantitative determination of grain blast in grams.