DLLME-UPLC-MS/MS法测定豆芽中6-苄基腺嘌呤残留

Determination of 6-Benzyl Adenine Residues in Sprouts by Dispersive LiquidLiquid Micro Extraction-Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

建立豆芽中6-苄基腺嘌呤残留的分散液液微萃取-超高效液相色谱-串联质谱检测方法。试验采用富集因子评价萃取效率,考察影响萃取效率的主要因素,主要有萃取剂类型及其用量、分散剂类型及其用量、超声辅助萃取时间、盐浓度、p H等。结果表明,在最佳萃取条件下(四氯乙烷100μL、甲醇1 mL、水5 mL、氯化钠1.5 g/mL、超声时间10 min),该法对6-苄基腺嘌呤具有较高的富集能力,富集因子为39.1~44.3。方法检出限为0.5μg/kg,定量低限为1.5μg/kg。在0.2~100 ng/mL范围内峰强度与质量浓度的线性关系良好(r>0.99)。方法的回收率为68.4%~70.3%。该方法具有简单、快速、稳定、灵敏度高和使用有机试剂少等特点,适合于实验室快速筛查检测。

A method for determination of 6-benzyl adenine residues in bean sprouts by dispersive liquid-liquid micro extraction-ultra high performance liquid chromatography tandem mass spectrometry was established.The extraction efficiency was evaluated by enrichment factor,and the main factors affecting the extraction efficiency were investigated and optimized,including the type and dosage of the extractant,the type and dosage of dispersant,the time of ultrasonic assisted extraction,the concentration of salt and the pH.The results showed that under the optimal extraction condition(100μL tetrachloroethane,1 mL methanol,5 mL water,1.5 g/mL sodium chloride,and ultrasonic 10 min),the method had a high enrichment capacity of6-benzylamine adenine,and the enrichment factor was between 39.1 and 44.3.The detection limit of the method was up to 0.5μg/kg,and the quantitative low limit was 1.5μg/kg.The linear relationship between peak intensity and mass concentration in the range of 0.2 to 100 ng/mL was good(r>0.99).The recovery rate of the method was 68.4%-70.3%.The method was simple,fast,stable,accurate and sensitive,and had few organic reagents.It was suitable for the laboratory to test the sprout samples.