摘要
建立了马铃薯中α-萘乙酸甲酯(MENA)的QuEChERS-高效液相色谱测定方法。样品用乙腈提取,经乙二胺-N-丙基硅烷(PSA)、十八烷基键合硅胶(C_18)和无水Mg SO_4分散固相萃取净化后,采用C_18色谱柱分离,以乙腈和pH 3的磷酸水溶液(46:54,V/V)为流动相进行洗脱,二极管阵列检测器在223 nm下检测。结果表明,MENA在0.025~2.0 mg/L的范围有良好的线性关系,相关系数为0.9999,检出限(LOD,S/N=3)为0.018 mg/L,方法的加标回收率达87.9%~100.3%,日内精密度在2.0%~6.3%之间,日间精密度在3.2%~6.4%之间。
A method for the determination of 1-naphthaleneacetic acid methyl ester （MENA） in potatoes by high performance liquid chromatography （HPLC） coupled with QuEChERS sample preparation was established. MENA was initially extracted from potato samples by aeetonitrile, and then purified using dispersive solid-phase extraction with anhydrous MgSO4, C18 and primary secondary amine （PSA）. After that the purified extract was separated on an Agilent Zorbax SB C18 column （250 mm ×4. 6 mm, 5μm） with mobile phase composed of acetonitrile and phosphoric acid aqueous solution （pH 3,46：54, V/V）, at a flow rate of 1.0 mL/min. MENA was analyzed by diode array detector operated at a wavelength of 223 nm. The calibration curve of MENA showed a good linearity in the range of 0. 025 ~ 2. 0 mg/L with a correlation coefficient （r2） of 0. 9999, and the limit of detection （ LOD, SIN = 3） was 0. 018 mg/kg. At the 4 spiked levels of 0. 05, 0. 25, 0. 5 and 1.5 mg/kg, average recoveries of the method varied between 87.9% and 100. 3% , while intra-day and inter-day relative standard deviations （RSDs） ranged from 2. 0% to 6.3% and 3.2% to 6. 4%, respectively.
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第2期131-135,共5页
Chinese Journal of Analysis Laboratory
基金
十二五973课题(2013CB127101)资助
