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  

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

作　　者：张婧[1] 万慧慧[1] 张华[1] 

机构地区：[1]大连理工大学化工与环境生命学部化学分析测试中心,辽宁大连116024

出　　处：《分析科学学报》2017年第3期387-390,共4页Journal of Analytical Science

基　　金：国家自然科学基金(No.21505014);大连理工大学引进人才科研专题(No.DUT15RC(4)13)

摘　　要：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(150×2.1mm,5μm)分离,以甲醇(A)/0.1%甲酸-5mmol/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2.63~675.00ng/mL范围内线性关系良好,相关系数R2>0.999。定量检测限为0.66ng/mL。氯吡脲在10、25、50ng/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。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（150×2.1mm,5μm） 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.

关 键 词：基质分散固相萃取 高效液相色谱-质谱联用 植物生长调节剂 氯吡脲 

分 类 号：O657.63[理学—分析化学]