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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 establish a method for the determination of memory-deficient molluscicides-domoic acid (DA) residues in scallop by QuEChERS sample preparation and high performance liquid chromatography (HPLC). Methods QuEChERS sample preparation was used to pretreat the sample, that is, the sample was extracted with methanol: acetonitrile: water = 6: 3: 1 (v: v: v), C18 powder was purified by reversed-phase high performance liquid chromatography and detected at 242 nm , Matrix matching calibration curve external standard method. Results The limit of quantitation (LOQ) of the method was 1.8 μg / g. The linearity of DA was linear over the concentration range of 0.72-30.00 μg / mL (r = 0.9998). At the concentration of 1.8-6.0 μg / g Within the range, the average recovery rate is about 90% and the relative standard deviation (RSD) is less than 5%. Conclusion The lower limit of detection method in this experiment meets the limit requirement of DA 20 μg / g. The method has the advantages of simple steps, strong operability, time saving, less reagent usage, high accuracy, good precision and fast and high efficiency.