QuEChERS法联合高效液相色谱法快速检测扇贝中的软骨藻酸

Rapid detection of domoic acid in scallops by QuEChERS method coupled with high performance liquid chromatography

目的利用QuEChERS样品制备结合高效液相色谱法建立测定扇贝中记忆缺失性贝类毒素—软骨藻酸(domoic acid,DA)残留的检测方法。方法 QuEChERS样品制备法进行样品前处理,即样品经甲醇:乙腈:水=6:3:1(v:v:v)提取,C18粉末净化,反相高效液相色谱分离,242 nm波长下检测,基质匹配校准曲线外标法定量。结果方法的检测低限(limit of quantitation,LOQ)为1.8μg/g,DA在0.72~30.00μg/m L浓度范围内线性良好(相关系数r=0.9998),在1.8~6.0μg/g添加浓度范围内,平均回收率为90%左右,相对标准偏差(relative standard deviation,RSD)小于5%。结论本实验建方法检测低限完全满足DA 20μg/g的限量要求,且步骤简单、可操作性强、节省时间、试剂用量少、准确度高、精密度好,具有快速高效的特点。

Objective To established a method to detect domoic acid residues in scallops by the sample processing method of QuEChERS in combination with high performance liquid chromatography (HPLC). Methods Samples were cleaned up by QuEChERS with extracting by methanol:acetonitrile:water=6:3:1 (v:v:v), and purified by C18 powder, separated by reversed phase high performance liquid chromatography and detected at wave length of 242 nm, and quantified by the matrix matching calibration curve external standard method of matrix matching calibration curve at last. Results The limit of quantitative was 1.8μg/g, working curve correlation coefficient was 0.9998 at the linear range of 0.72~30.00μg/mL, the recovery rate was higher than 90% at the spiking concentration range of 1.8~6.0 μg/g, and relative standard deviation (RSD) was less than 5%. Conclusion This method with a fast speed and a high sensitivity and exactitude can satisfy the limit of detection of DA 20μg/g.