QuEChERS-高效液相色谱串联质谱法快速筛查分析食品中五氯酚酸钠残留

Rapid screening analysis of pentachlorophenol sodium residue in foods by QuEChERS-high performance liquid chromatography tandem mass spectrometry

中文关键词:  五氯酚酸钠  QuEChERS  高效液相色谱串联质谱法  电喷雾离子化  多反应监测

英文关键词:pentachlorophenol sodium  QuEChERS  high performance liquid chromatography-tandem mass spectrometry  electrospray ionization  multiple reaction monitoring

中文摘要:

      目的 建立动物性食品中五氯酚酸钠(pentachlorophenol sodium, PCP-Na)残留的高效液相色谱串联三重四级杆质谱(high performance liquid chromatography tandem mass spectrometry, HPLC-MS/MS)快速筛查分析方法。方法 样品采用80%乙腈水溶液提取, 提取液经QuEChERS净化管净化、氮吹浓缩并以40%甲醇定容。以甲醇-5 mmol/L乙酸铵水溶液为流动相梯度洗脱, 经Waters Acquity UPLC HSS T3(2.1 mm×100 mm, 1.7 μm)色谱柱分离, 质谱采用负离子电喷雾离子化(ESI-)、多反应监测(multiple reaction monitoring, MRM)模式定性和定量。结果 方法线性范围为0.3~20.0 μg/L(r>0.999), 对于畜禽类动物性食品, 加标浓度为2.0 μg/kg和 10.0 μg/kg时回收率范围为68.5%~99.3%, 相对标准偏差为1.7%~16.2%(n=6)。方法检出限为0.1 μg/kg, 定量限为0.3 μg/kg。结论 本方法样品前处理快速、简单, 检测灵敏度高、选择性好, 适用于大批量动物性食品样品中痕量五氯酚酸钠残留的快速筛查分析。

英文摘要:

      Objective To establish a rapid screening analysis method for pentachlorophenol sodium (PCP-Na) residue in animal-origin foods by QuEChERS-high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with 80% acetonitrile aqueous solution, the extract was purified by QuEChERS purification tube, concentrated by nitrogen blowing and fixed with 40% methanol. Methanol-5 mmol/L ammonium acetate aqueous solution was used as mobile phase for gradient elution, and samples were separated by Waters Acquity UPLC HSS T3 (2.1 mm×100 mm, 1.7 μm) column. The mass spectrometry was qualitative and quantitative by negative ion electrospray ionization (ESI-) and multiple reaction monitoring (MRM). Results PCP had good linear relationships in the range of 0.3~20.0 μg/L with the correlation coefficient higher than 0.999. For animal-original food samples, recoveries ranged from 68.5% to 99.3% with relative standard deviations (RSDs) of 1.7%~16.2% (n=6). The limits of detection (LOD) (S/N=3) and limits of quantification (LOQ) (S/N=10) were 0.1 μg/kg and 0.3 μg/kg, respectively. Conclusion The proposed method is of rapid, simplicity, high sensitivity and good selectivity, which is suitable for rapid PCP-Na residue screening analysis of large quantities animal-origin foods.