高效液相色谱法测定油菜籽中草除灵乙酸

Determination of benazolin in rapeseed by HPLC

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。

To date, there is still no established method on the detection of benazolin residues. In this paper, a method for the determination of benazolin in rapeseed by HPLC is described. The analytes were extracted from samples using ammonia and methanol, purified by MAX solid phase extraction column, and then analyzed using HPLC by UV detector with a Cls column （250 mm × 4.6 mm, 5 μm）. All the analytes were quantified by the external standard. The calibration curve was linear between the peak area and the mass concentration of benazolin from 0. 05 to 1.00 mg/L with the correlation coefficient of 0. 999. The limit of quantification （LOQ） of this method is 0. 1 mg/kg. The results from the test of three concentration levels （0. 1 mg/kg, 0.2 mg/kg, 0.4 mg/kg, every level reapeated six times ） by four different persons show that overall recoveries were between 75% and 100% , and the relative standard deviation was 1.1% -6. 9%. According to the validation by four laboratories, the repeatability standard deviations were in the range of 3.6% ~ 6.9%, and the reproducibility standard deviation were in the range of 5.8 % - 17 % , satisfying the relevant legal and regulatory requirements.