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作 者:宋东晓 SONG Dongxiao(Ningde Food and Drug Inspection and Testing Center,Ningde 352000,China)
机构地区:[1]宁德市食品药品检验检测中心,福建宁德352000
出 处:《食品安全导刊》2023年第20期67-70,共4页China Food Safety Magazine
摘 要:通过对比QuEChERS法与传统固相萃取法(Solid-Phase Extraction,SPE)两种前处理方法,建立高效液相色谱-串联质谱法测定猪肉中五氯酚残留量。本实验对猪肉中五氯酚钠检出限、定量限、准确度、回收率、基质效应进行考察分析。对比QuEChERS和SPE两种前处理方法,猪肉中五氯酚钠标液在0.5~25.0 ng·mL^(-1)线性关系良好,相关系数均大于0.999,检出限均为0.1μg·kg^(-1),定量限均为0.5μg·kg^(-1)。在0.5μg·kg^(-1)、1.0μg·kg^(-1)、5.0μg·kg^(-1)3水平浓度下进行加标回收,SPE法回收率在107.61%~113.58%,相对标准偏差为3.72%~6.16%,QuEChERS法回收率在88.03%~113.57%,相对标准偏差为2.05%~5.99%。SPE和QuEChERS法中,五氯酚钠在猪肉中ME值0.264~0.541,均表现出强基质效应。这两种前处理方法差异不明显,均能满足猪肉中五氯酚钠残留量的检测需求,但QuEChERS法更高效。A quantitative method for the determination of sodium pentachlorophenol in pork by LC-MS was established by comparing the QuEChERS method with the traditional solid-phase extraction method for pre-treatment.In the experiment,the detection limit,quantification limit,accuracy,recovery rate and matrix effect of sodium pentachlorophenolate in pork were investigated and analyzed.The linear relationship of sodium pentachlorophenol in two pre-processing methods was good in the concentration range of 0.5~25.0 ng·mL^(-1),the correlation coefficient was greater than 0.999,the detection limit of was 0.1μg·kg^(-1),the quantification limit was 0.5μg·kg^(-1).At the spiked concentrations of 0.5μg·kg^(-1),1.0μg·kg^(-1) and 5.0μg·kg^(-1),the recovery was 107.61%~113.58%in SPE,and the corresponding RSD was 3.72%~6.16%.In QuEChERS,the recovery was 88.03%~113.57%,and the corresponding RSD was 2.05%~5.99%.In the SPE and QuEChERS methods,the ME values of sodium pentachlorophenol in pork ranged from 0.264 to 0.541,both of the two pre-processing methods can meet the detection of sodium pentachlorophenolate residue in pork,but the QuEChERS method is more efficient.
关 键 词:猪肉 五氯酚钠 高效液相色谱-串联质谱法 QUECHERS 传统固相萃取法(SPE)
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