同位素内标法测定水产品中五氯酚残留量的研究  

Determination of Pentachlorophenol Residues in Aquatic Products Using Isotope Internal Standard Method

作　　者：吴芳海 WU Fanghai(Quanzhou Institute for Food and Drug Control,Quanzhou 362000,China)

机构地区：[1]泉州市食品药品检验所,福建泉州362000

出　　处：《食品科技》2024年第12期328-332,共5页Food Science and Technology

基　　金：福建省市场监督管理局科技项目(FJMS2021034)。

摘　　要：目的:建立同位素内标法测定水产品中五氯酚残留量的分析方法。方法:样品经乙腈提取,提取溶液用新型材料Cleanert LipoNo吸附除脂,经ACQUITY UPLC?BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,以5 mmol/L乙酸铵溶液和甲醇为流动相梯度洗脱,流速0.25 mL/min,柱温30℃,进样量5μL。采用电喷雾离子源,负离子多反应监测模式,内标法定量分析。结果:五氯酚在添加量为1.0、2.0、10.0μg/kg时,回收率为86.6%~113.4%,相对标准偏差为0.9%~3.2%。在1.0~20.0 ng/mL浓度范围内线性关系良好,相关系数为0.9998,检出限为0.5μg/kg。结论:该方法前处理操作简单便捷,利用内标法定量,灵敏度高、重复性好、结果准确,适用于不同基质水产品中五氯酚残留量的定量测定。Objective:In order to establish an analytical method for the determination of pentachlorophenol residues in aquatic products using isotope internal standard method.Method:The samples were extracted with acetonitrile,and the extract solution was defatted using the novel material Cleanert LipoNo.The separation was achieved using an ACQUITY UPLC?BEH C_(18)(2.1 mm×100 mm,1.7μm)chromatographic column,with a gradient elution of 5 mmol/L ammonium acetate solution and methanol as the mobile phase,the flow rate was 0.25 mL/min,the column temperature was 30℃,and the injection amount was 5μL.The electrospray ionization source(ESI)and negative ion multiple reaction monitoring mode were employed,and internal standard method were used for quantitative analysis.Results:When the addition levels of pentachlorophenol were 1.0,2.0,10.0μg/kg,the recovery rates ranged from 86.6%to 113.4%,and the relative standard deviations ranged from 0.9%to 3.2%.The linear relationship was good in the concentration range of 1.0 ng/mL to 20.0 ng/mL,with a correlation coefficient of 0.9998 and the limit of detection was 0.5μg/kg.Conclusion:This method with internal standard method for quantification has a simple and convenient pre-treatment process,high selectivity,good repeatability,and could get accurate results.It is suitable for the quantitative determination of residual pentachlorophenol in different aquatic products matrix.

关 键 词：五氯酚 水产品 内标法 

分 类 号：TS207.53[轻工技术与工程—食品科学]