超高效液相色谱-串联质谱法测定柞蚕中苦参碱和氧化苦参碱残留量的研究

Determination of Matrine and Oxymatrine Residues in Tussah Silkworm by Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

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 100A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。

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 2.6μm Biphenyl 100Acolumn(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 0.05μg/kg,and the detection limit of oxymatrine was 0.1μg/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.