超高效液相色谱-串联质谱法测定草鱼和中华绒螯蟹中五氯酚酸钠残留量

Determination of pentachlorophenol sodium residues in Ctenopharyngodon idella and Eriocheir sinensis by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  固相萃取  水产品  五氯酚酸钠

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  solid phase extraction  aquatic products  pentachlorophenol sodium

中文摘要:

      目的 建立水产品中五氯酚酸钠残留量的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测方法。方法 样品前处理经由80%乙腈水(含5%三乙胺)提取, 上清液经过Waters Oasis MAX固相萃取柱柱净化, 4%甲酸甲醇溶液洗脱后, 采用UPLC-MS/MS的方法进行检测, 使用Waters XBridge C18色谱柱(100 mm×2.10 mm, 3.50 μm); 流动相为A: 0.1%甲酸水(含5 mmol/L醋酸铵), B: 乙腈, 外标法定量, 并对两种基质草鱼肌肉及中华绒螯蟹可食部分中五氯酚酸钠回收率进行考察。结果 草鱼和中华绒螯蟹中五氯酚酸钠残留检测在线性范围0.2~8.0 ng/mL内具有良好的线性关系, 相关系数r2>0.999, 检出限为0.5 μg/kg, 定量限为1.0 μg/kg, 添加浓度1.0、2.0和10.0 μg/kg下的回收率均在77.0%~105%之间, 批内相对标准偏差2.51%~7.62% (n=6), 批间相对标准偏差3.36%~6.48% (n=3)。结论 用本方法测定草鱼和中华绒螯蟹中的五氯酚酸钠残留量, 灵敏度高, 准确度和精密度良好, 操作简便, 适用于水产品中五氯酚酸钠残留量的检测。

英文摘要:

      Objective To develop an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of pentachlorophenol sodium residues in aquatic products. Methods The sample preparation involved extraction with 80% acetonitrile in water containing 5% triethylamine, followed by purification using Waters Oasis MAX solid-phase extraction cartridges. After elution with a 4% formic acid in methanol solution, the pentachlorophenol sodium was analyzed by UPLC-MS/MS using a Waters XBridge C18 column (100 mm × 2.10 mm, 3.50 μm). The mobile phases consisted of A: 0.1% formic acid in water (containing 5 mmol/L ammonium acetate) and B: acetonitrile. Quantification was carried out using the external standard method. The recovery of pentachlorophenol sodium in the muscle of Ctenopharyngodon idella and the eatable part of Eriocheir sinensis matrices was examined. Results The linear range of the pentachlorophenol sodium residue detection method in Ctenopharyngodon idella and Eriocheir sinensis was 0.2 to 8.0 ng/mL (r2>0.999). The limit of detection was 0.5 μg/kg and limit of quantification was 1.0 μg/kg, respectively. The recoveries at spiking levels of 1.0, 2.0, and 10 μg/kg were within the range of 77.0% to 105%. Intra-assay relative standard deviations ranged from 2.51% to 7.62% (n=6), and inter-assay relative standard deviations ranged from 3.36% to 6.48% (n=3). Conclusion The developed UPLC-MS/MS method for the determination of pentachlorophenol sodium residues in Ctenopharyngodon idella and Eriocheir sinensis matrices is highly sensitive, accurate, and precise, with good repeatability and reproducibility, and is therefore suitable for the detection of pentachlorophenol sodium residues in aquatic products.