高效液相色谱法测定棉菜籽中甲萘威残留量

Determination of Carbaryl Residue in Cotton Rapeseed by HPLC

建立高效液相色谱法检测棉菜籽中甲萘威的分析方法。样品经乙酸甲醇旋涡提取、静止后,加入QuECHERS试剂振荡后取上清液氮气吹干,定容,通过ASB-C18色谱柱分离,流动相采用甲醇+水(80+20,V/V),流速1.0 mL·min^(-1),柱温40℃,进样量10μL,在280 nm波长下测定。结果表明,在0.10~10 mg·L^(-1)范围内,线性方程相关系数为0.9998。在添加量为0.500~1.500 mg·kg^(-1)时,回收率为82.9%~91.9%,测定结果的相对标准偏差(n=6)在2.17~4.25%。检出限为0.1 mg·kg^(-1),定量限为0.5 mg·kg^(-1)。该试验方法具有操作便捷、结果准确可靠且重现性好等优点。

To establish a HPLC method for the determination of Carbaryl in Cotton Rapeseed.After the samples were extracted by acetic acid and methanol vortex,the liquid nitrogen was dried with QuEChers reagent,and then the liquid nitrogen was dried with constant volume.The liquid nitrogen was separated on an ASB-C18 column.The mobile phase was methanol+water(80+20,V/V)at the flow rate of 1.0 mL·min^(-1).The column temperature was 40℃,the sample size was 10μL,and the sample size was determined at 280 nm wavelength.The results show that the correlation coefficient of the linear equation is 0.9998 in the range of 0.10~10 mg·L^(-1).The recoveries were in the range of 82.9%~91.9%,and the relative standard deviations(n=6)were in the range of 2.17%~4.25%when the supplemental level was 0.500~1.500 mg·kg^(-1).The limit of detection was 0.1 mg·kg^(-1) and the limit of quantification was 0.5 mg·kg^(-1).This test method has the advantages of convenient operation,accurate and reliable results and good reproducibility.