液相色谱-串联质谱法分析洋葱中甲苯磺丁脲含量

Analysis of tolbutamide content in onion by liquid chromatography-tandem mass spectrometry

通过液相色谱-串联质谱(LC-MS/MS)法建立一种检测洋葱中甲苯磺丁脲含量的方法,并对不同地区洋葱中甲苯磺丁脲含量进行分析。结果表明:建立的方法提取溶剂为乙腈、色谱柱为Waters ACQUITY UPLCBEH Phenyl(50 mm×2.1 mm, 1.7μm)、流动相为10 mmol/L甲酸铵-乙腈溶液、流动相流速为0.3 mL/min、等度淋洗方式。当甲苯磺丁脲在2.0~100.0 ng/mL范围内时线性关系良好,回收率为98.9%~103.1%、相对标准偏差为0.44%~1.52%、检出限为0.5μg/kg、定量限为2.0μg/kg。对全国8个主产区的洋葱进行分析发现,甘肃酒泉洋葱的甲苯磺丁脲含量最高。

A method for detecting the content of tolbutamide in onions was established by liquid chroma-tography-tandem mass spectrometry(LC-MS/MS),and the content of tolbutamidea in onions from dif-ferent regions was analyzed.The results showed that the established method used acetonitrile as the ex-traction solvent and the chromatographic column was Waters ACQUITY UPLC BEH Phenyl(50 mm×2.1 mm,1.7μm),mobile phase of 10 mmol/L ammonium formate-acetonitrile solution,mobile phase flow rate of 0.3 mL/min,and equal degree elution method.When tolbutamide was in the range of 2.0-100.0 ng/mL,the linear relationship was good,with recovery rate of 98.9%-103.1%,relative standard deviation of 0.44%-1.52%,detection limit of 0.5μg/kg,and quantification limit of 2.0μg/kg.Analysis of onions from 8 major production areas across the country revealed that Jiuquan on-ions in Gansu Province had the highest content of tolbutamide.