基质分散固相萃取-高效液相色谱/串联质谱法检测红薯中氯吡脲

建立了分散固相萃取-高效液相色谱/串联质谱法测定红薯中氯吡脲含量的分析方法.样品经分散剂(硅胶,C18HC)研磨分散提取,甲醇洗脱.采用Thermo Hypersil Gold C18色谱柱(150×2,1 mm,5μm)分离,以甲醇(A)/0.1％甲酸-5 mmol/L甲酸铵(B)作为流动相,梯度洗脱,采用串联质谱在正离子扫描方式下,通过选择反应模式定量分析,外标法定量.氯吡脲在2.63～675.00 ng/mL范围内线性关系良好,相关系数R2＞0.999.定量检测限为0.66 ng/mL.氯吡脲在10、25、50 ng/g三个浓度水平的添加回收率在70％～130％之间.该方法操作简单、准确,适用于红薯中氯吡脲的定量检测.

Detection of Forchlorfenuron in Batatas by Matrix Solid-Phase Dispersive Extraction and High Performance Liquid Chromatography-Tandem Mass Spectrometry

A sample method based on the matrix solid-phase dispersive(MSPD) extraction coupled with high performance liquid chromatography-tandem mass spectrometry was developed for the determination of forchlorfenuron in batatas.The samples were dispersed with dispersant materials(silica and C18HC)by grinding,and then extracted with methanol.The determination was carried out on a Thermo Hypersil Gold C18 column(150 × 2.1 mm,5 μm) in gradient elution with mobile phases of methanol and 5 mmol/L ammonium formate(containing 0.1％ formic acid).The compound was detected with high performance liquid chromatography-tandem mass spectrometry operated in the positive electro-spray ionization using selected reaction monitoring mode,and the quantification was performed using external standard calibration with the correlation coefficient larger than 0.999.The linear ranges of forchlorfenuron were between 2.63 ng/mL and 675.00 ng/mL.The LOQ of the plant growth regulator was 0.66 ng/mL.The spiked recoveries at levels of 10 ng/g,25 ng/g and 50 ng/g of forchlorfenuron were in the range of 70％-130％.This method has advantages of simple operation and good accuracy,and can be used for quantitative determination of forchlorfenuron in batatas.