萘乙酸残留量的液相色谱法测定

在小麦、棉花、苹果等反复试验的基础上,建立了萘乙酸残留量定量检测的液相色谱法。样品经甲醇提取,过SPE C18小柱净化,采用150mm×4.6mm,C18不锈钢色谱柱,以甲醇+水+冰乙酸(体积比50∶50∶0.2)为流动相,流速为1.0mL/min,检测波长280nm,外标法定量进行HPLC测定。方法的线性范围在0.01～1.00mg/L,线性方程Y=3386.4X–105.96,相关系数0.9999;最小检出量为0.001ng,最低检出浓度0.001mg/kg,回收率为80.6%～101.2%。

Determination of Naphthyl-acetic Acid Residues by HPLC

On the base of repetitive experiments in wheat,cotton and apple,the high performance liquid chromato-graphy was established on the quantitative determination of naphthyl-acetic acid residual content.Samples were extracted with methyl alcohol,clean-up in SPE C18 small column.The analysis was then performed on a C18 stainless steel column(150 mm×4.6 mm i.d.) with mixture of methanol+water+acetic acid(50∶50∶0.2,by vol)as the mobile phase at a flow rate of 1.0 mL/min and the ultraviolet detection wavelength 280 nm.The method was fast and accurate with a linear correlation of 0.999 9 in the range of 0.01 mg/L to 1.00 mg/L,the linearity equation was Y=3 386.4 X–105.96,average append recoveries was ranged from 80.6% to 101.2%,LOD was 0.001 ng and LOQ was 0.001 mg/kg.