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建立了一种油菜籽中草除灵乙酸的液相色谱检测方法。样品中残留的草除灵乙酸,用氨水和甲醇混合溶液提取,经MAX固相萃取柱净化,以C_(18)色谱柱(250 mm×4.6 mm,粒径5μm)分离,液相色谱-紫外检测法测定,外标法定量。在0.05~1.00 mg/L范围内,草除灵乙酸的峰面积与质量浓度呈良好的线性关系,相关系数r=0.999。方法的定量限(LOQ)为0.1mg/kg。对油菜籽空白样品进行了4位不同检测人员、3个水平(0.1,0.2,0.4 mg/kg)和6次重复的添加回收实验,平均回收率为75%~100%,相对标准偏差为1.1%~6.9%。同时又进行了4个实验室间的重复性和再现性评价,结果表明实验室内重复性相对标准差为3.6%~6.9%,实验室间再现性相对标准差为5.8%~17%,满足相关法律法规的要求。
A liquid chromatography method was established for the determination of ramie grass and ramification acetic acid. Residues of acetic acid in the samples were extracted with a mixture of ammonia and methanol, purified by MAX solid-phase extraction, and separated on a C 18 column (250 mm × 4.6 mm, particle size 5 μm). Liquid chromatography-ultraviolet Detection method, external standard method. In the range of 0.05-1.00 mg / L, there was a good linear relationship between the peak area and the concentration of trimethoprim with the correlation coefficient r = 0.999. The method has a limit of quantitation (LOQ) of 0.1 mg / kg. The rapeseed blank samples were subjected to 4 different tests, 3 recovery levels (0.1, 0.2, 0.4 mg / kg) and 6 replicates. The average recoveries ranged from 75% to 100% and the relative standard deviations were 1.1 % ~ 6.9%. At the same time, the repeatability and reproducibility evaluation of four laboratories was also conducted. The results showed that the relative standard deviation of repeatability in laboratory was 3.6% ~ 6.9% and the relative standard deviation of reproducibility in laboratory was 5.8% ~ 17% Relevant laws and regulations requirements.