Li Cheng, Suo Ran, Wang Fengchi, Ma Hongying
College of Food Science, Agricultural University of Hebei, Baoding 071000, China.
Se Pu. 2008 Nov;26(6):726-30.
A method for the simultaneous determination of six pesticides in adzuki beans by high performance liquid chromatography-electrospray ion trap tandem mass spectrometry was developed and evaluated. The sample was extracted with 0.1 mol/L NH4HCO3 (pH 5)-methanol (70 : 30, v/v). The extract was partitioned with dichloromethane, and cleaned up with gel permeation chromatography. The separation was performed on an Inertsil ODS-3 column (150 mm x 2.1 mm, 5 microm) with the gradient elution of methanol and 1% acetic acid as mobile phase. The identification and quantification were performed by electrospray ion trap mass spectrometry with selected ion monitoring mode. The calibration curves of imidazolinone herbicides showed good linearities in the range of 10 - 200 microg/L (5 -100 microg/L for imazaquin) with the correlation coefficients between 0.998 7 and 0.999 7. The limits of detection ranged between 0.2 microg/kg and 0.5 microg/kg (S/N = 3). The average recoveries of six imidazolinone herbicides spiked in adzuki beans ranged between 81.6% and 99.4% (n = 6) with the relative standard deviations of 3.1% -7.8%. The method has been used for the determination of 6 imidazolinone herbicides simultaneously in adzuki beans with easy operation, high accuracy and good precision.
建立并评估了一种用高效液相色谱-电喷雾离子阱串联质谱法同时测定小豆中6种农药的方法。样品用0.1 mol/L碳酸氢铵(pH 5)-甲醇(70:30,v/v)提取。提取物用二氯甲烷分配,并用凝胶渗透色谱法净化。在Inertsil ODS-3柱(150 mm×2.1 mm,5 µm)上以甲醇和1%乙酸为流动相进行梯度洗脱分离。通过电喷雾离子阱质谱法在选择离子监测模式下进行鉴定和定量。咪唑啉酮类除草剂的校准曲线在10 - 200 μg/L范围内呈良好线性(咪草喹为5 -100 μg/L),相关系数在0.998 7至0.999 7之间。检测限在0.2 μg/kg至0.5 μg/kg之间(S/N = 3)。在小豆中添加6种咪唑啉酮类除草剂的平均回收率在81.6%至99.4%之间(n = 6),相对标准偏差为3.1% -7.8%。该方法已用于同时测定小豆中的6种咪唑啉酮类除草剂,操作简便,准确度高,精密度好。