Aoyagi Mitsutoshi, Chiba Masahiro, Kakimoto Youichiro, Nemoto Satoru
Hokkaido Institute of Public Health.
Shokuhin Eiseigaku Zasshi. 2016;57(6):201-206. doi: 10.3358/shokueishi.57.201.
A method for the determination of diphenylamine in agricultural products was developed. Diphenylamine was extracted with acetonitrile from a sample under an acidic condition, passed through a C18 cartridge column, re-extracted with n-hexane, cleaned up on a PSA cartridge column, determined by HPLC with fluorescence detector and confirmed by liquid chromatography with tandem mass spectrometry. Average recoveries (n=5) from brown rice, corn, soybeans, potato, cabbage, eggplant, spinach, orange, apple and green tea were in the range from 76.7 to 94.9%, and the relative standard deviations were from 0.6 to 5.8% at concentrations equal to the maximum residue limits (MRLs). The quantification limits were 0.01 mg/kg, which is the uniform limit in the positive list system for agricultural chemical residues in food in Japan.
建立了一种测定农产品中 diphenylamine 的方法。在酸性条件下,用乙腈从样品中提取 diphenylamine,通过 C18 柱,再用正己烷重新提取,在 PSA 柱上净化,用带荧光检测器的高效液相色谱法测定,并用液相色谱 - 串联质谱法确证。糙米、玉米、大豆、马铃薯、卷心菜、茄子、菠菜、橙子、苹果和绿茶的平均回收率(n = 5)在 76.7%至 94.9%之间,在等于最大残留限量(MRLs)的浓度下,相对标准偏差为 0.6%至 5.8%。定量限为 0.01 mg/kg,这是日本食品中农业化学品残留肯定列表制度中的统一限量。