摘要
研究建立了禽蛋中五氯酚及其钠盐的液相色谱-串联三重四极杆质谱测定方法。样品经体积分数5%三乙胺的乙腈-水溶液(7:3,V/V)提取,混合型阴离子固相萃取柱净化,经ACQUITY UPLC BEH C_(18)(100 mm×2.1 mm,1.7μm)色谱柱分离,以5 mmol/L乙酸铵(含0.1%甲酸)溶液和乙腈作为流动相,进行梯度洗脱,采用多反应监测负离子模式监测,基质匹配标准曲线外标法定量。在该优化条件下,五氯酚及其钠盐在1.0-20 ng/mL浓度范围内线性关系良好,相关系数均大于0.998,检出限为0.5μg/kg,定量限为1.0μg/kg。在不同浓度添加水平下(1.0、2.0、5.0μg/kg),平均回收率为74.0%-101.3%,相对标准偏差为0.78%-6.56%(n=6)。该方法简单、高效、准确,提取液经冷冻处理后避免了净化时固相萃取柱堵塞情况出现,缩短实验时间,优化后的实验方法适用于禽蛋中五氯酚及其钠盐的残留检测。
A high liquid chromatography-tandem mass spectrometry method with solid phase extraction was established for the determination of pentachlorophenol and its sodium salt residues in poultry eggs.The sample was extracted by 5%triethylamine acetonitrile-water solution(7:3,V/V),purified by mixed anionic solid phase extraction column,and separated on an ACQUITY UPLC BEH Cis column(100 mm×2.1 mm,1.7μm)using 5 mmol/L ammonium acetate(containing 0.1%formic acid)solution and acetonitrile as mobile phase for gradient elution,and then determined by tandem mass spectrometry in negative ESl modes under multiple reaction monitoring(MRM).The matrix matched calibration curve method was used to further suppress the matrix effect.Under the optimized conditions,the developed method showed a good linearityin the range of 1.0-20.0 ng/mL,the correlation coefficient was greater than 0.998,the detection limit was 0.5μg/kg,the quantitation limit was 1.0μg/kg.The average recovery was 74.0%-101.3%,and the relative standard deviation was 0.78%-6.56%(n=6).The method is simple,efficient and accurate.After the extraction solution was frozen,the blockage of the solid phase extraction column during purification was avoided,and the experiment time was shortened.The optimized method was applicable to the residue detection of pentachlorophenol and its sodium salt in poultry eggs.
作者
李星
林立
王浩
王羽
李冬梅
史海良
张丽华
陈昱洁
LI Xing;LIN Li;WANG Hao;WANG Yu;LI Dongmei;SHI Hailiang;ZHANG Lihua;CHEN Yujie(Beijing Food Inspection and Research Institute(Beijing Food Safety Monitoring and Risk Assessment Center),Key Laboratory of Key Technologies of Major Comprehensive Guarantee of Food Safety for State Market Regulation,Beijing 100094,China)
出处
《食品科技》
CAS
北大核心
2023年第10期270-275,共6页
Food Science and Technology
关键词
液相色谱-串联质谱法
固相萃取
禽蛋
五氯酚及其钠盐
liquid chromatography-tandem mass spectrometry
solid phase extraction
poultry eggs
pentachlorophenol and its sodium salt
