期刊论文

Solid-phase extraction combined with high performance liquid chromatography for the determination of roxarsone in Oryza sativa

中文

湖南农业大学学报(自然科学版)

1007-1032

2021

47

4

482-486

10.13331/j.cnki.jhau.2021.04.018

湖南农业大学“双一流”建设项目（SYL201802021）；

本校为第一机构

通过对超声提取法中提取剂、固相萃取中淋洗液和洗脱剂、高效液相色谱中流动相的筛选,建立固相萃取–高效液相色谱定量检测水稻中洛克沙胂的方法。所建方法为:样品先经0.05 mol/L NaOH+20 g/L K_2HPO_4超声提取;再利用活化后的固相萃取小柱,依次采用1.5 mL 0.05 mol/L乙酸钠–甲醇溶液(pH=7)和1.5 mL甲醇淋洗及体积分数为13%的甲酸–甲醇溶液洗脱;最后利用以含0.3%甲酸的0.05 mol/L磷酸二氢钾溶液和甲醇(体积比80∶ 20)为流动相的高效液相色谱进行定量分析;该方法在洛克沙胂质量浓度为0.01~10.00 mg/mL时线性关系良好,相关系数大于0.999,检测限和定量限分别为20、67 ng/kg;洛克沙胂在水稻根、茎...

To develop a method for quantitative determination of roxarsone(ROX) in Oryza sativa, a group of conditions including extractant, leachate, eluant and mobile phase were tested. The results showed that the condition with extractant, 0.05 mol/L NaOH-20 g/L K_2HPO_4, included the activated solid phase extraction column, with the leachate 1.5 mL 0.05 mol/L CH3COONa-CH_3OH(pH=7) and 1.5 mL CH_3OH, and with the eluant 13% HCOOH-CH_3OH(V/V) solution, and the method of 0.05 mol/L K_2HPO_4 solution containing 0.3% HCOOH and CH_3OH(the volume ratio was 8...