高效液相色谱法测定水产品中4-己基间苯二酚

Determination of 4-hexylresorcinol in aquatic products by high performance liquid chromatography

建立了水产品中4-己基间苯二酚(4-HR)残留量测定的高效液相色谱-荧光法。样品经乙腈提取,浓缩后用流动相溶解残渣,正己烷脱脂净化,过滤后供高效液相色谱(HPLC)分析。色谱条件为:WondaSilC18柱(250mm×4.6mm,5μm);以甲醇-水(75:25,v/v)作为流动相,流速为1.0mL/min;荧光检测器激发波长为280nm,发射波长为310nm,外标法定量。结果表明:该方法在0.05～5.0μg/mL范围内线性关系良好,相关系数R2=0.9998。样品在0.1、0.2、1.0、5.0mg/kg加标水平时,平均回收率为90.9%～108.4%,相对标准偏差(RSD)为0.8%～8.1%(n=5)。方法定量限(LOQ)为0.1mg/kg。

A method for the determination of 4-hexylresorcinol in aquatic products was established by high performance liquid chromatography with fluorescence detection.The sample was extracted with acetonitrile and then the solvent extraction was evaporated to dryness.The residue was dissolved with the mobile phase followed by a clean-up step using n-hexane.The diluted solution was determined by HPLC.Chromatographic separation was carried out on a C18 column（250mm×4.6mm,5μm）with elution of methanol-water solution（75：25,v/v）at a flow rate of 1.0mL/min.The fluorescence detection was performed at an excitation wavelength of 280nm and an emission wavelength of 310nm.4-hexylresorcinol was quantified by the external standard method.The calibration curves showed good linearity in the concentrations range of 0.05 ~ 5.0μg/mL for the standard solutions.The correlation coefficents（R2）was 0.9998.The average recoveries were 90.9% ~ 108.4% at spiked levels of 0.1,0.2,1.0 and 5.0 mg/kg.The relative standard deviations（RSD,n=5）were 0.8% ~ 8.1%.The limit of quantification（LOQ）was 0.1mg/kg.