【摘要】 为建立超高效液相色谱-串联质谱法测定柞蚕中苦参碱、氧化苦参碱残留量分析方法，用80%乙腈水溶液(含0.2%氨水)超声提取样品，经分散固相萃取净化，以Kinetex 2.6μm Biphenyl 100?色谱柱(100 mm×3.0 mm)分离，0.1%甲酸水和0.1%甲酸甲醇为流动相梯度洗脱，电喷雾电离(ESI),正离子模式多反应监测(+MRM)下检测，外标法定量。结果表明，苦参碱、氧化苦参碱在0.1～50.0 ng/mL范围内呈良好的线性关系，相关系数r均大于0.999,加标回收率在64%～118%之间，相对标准偏差均小于11%,苦参碱检出限为0.05μg/kg,氧化苦参碱检出限为0.1μg/kg。该方法具有较高的灵敏度、准确度和重现性，可用于柞蚕中苦参碱、氧化苦参碱残留量的测定，并为相关产品中苦参碱、氧化苦参碱残留量检测提供了方法依据。更多还原

【Abstract】 To establish an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of matrine and oxymatrine residues in tussah silkworm, the sample was ultrasonically extracted with 80% acetonitrile aqueous solution(containing 0.2% ammonia) and purified by dispersive solid-phase extraction. It was separated on a Kinetex 2.6 μm Biphenyl 100 ? column(100 mm×3.0 mm), gradient eluted with 0.1% formic acid and 0.1% formic acid methanol, detected with electron spray ionization(ESI) and positive ion mode multiple reaction monitoring(+MRM), and quantified by external standard method. The results showed that the matrine and oxymatrine had a good linear relationship in the range of 0.1-50.0 ng/mL. The correlation coefficient r was greater than 0.999, and the recovery rate of standard addition was between 64% and 118%. The relative standard deviation was less than 11%, the detection limit of matrine was 0.05 μg/kg, and the detection limit of oxymatrine was 0.1 μg/kg. This method has high sensitivity, accuracy, and reproducibility, and can be used for the determination of matrine and oxymatrine residues in tussah silkworm. Also, it provides a method for the determination of matrine and oxymatrine residues in related products.更多还原