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

作　　者：娄晓祎 徐依琳 罗慧娟 王艺红[4] 黄宣运[1] 李水根 黄冬梅[1] 陈旭 LOU Xiao-Yi;XU Yi-Lin;LUO Hui-Juan;WANG Yi-Hong;HUANGXuan-Yun;LI Shui-Gen;HUANG Dong-Mei;CHEN Xu(Key Laboratory of Aquatic Product Quality and Safety Control of the Ministry of Agriculture and Rural Affairs,East China Sea Fishery Research Institute,Chinese Academy of Fishery Sciences,Shanghai 200090,China;College of Food Science and Technology,Shanghai Ocean University,Shanghai 201306,China;Institute of Food Science and Technology,Chinese Academy of Agricultural Sciences,Beijing 100193,China;Zhangzhou Fishery Technology Extension Station,Zhangzhou 363000,China;Fujian Fisheries Technology Extension Center,Fuzhou 350002,China)

机构地区：[1]中国水产科学研究院东海水产研究所,农业农村部水产品质量安全控制重点实验室,上海200090 [2]上海海洋大学食品学院,上海201306 [3]中国农业科学院农产品加工研究所,北京100193 [4]漳州市水产技术推广站,漳州363000 [5]福建省水产技术推广总站,福州350002

出　　处：《食品安全质量检测学报》2025年第4期78-85,共8页Journal of Food Safety and Quality

基　　金：上海科技兴农项目(2022-02-08-00-12-F01108)。

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,3.50μm);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0.5μg/kg,定量限为1.0μg/kg,添加浓度1.0、2.0和10.0μg/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。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,3.50μm).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 0.5μg/kg and limit of quantification was 1.0μg/kg,respectively.The recoveries at spiking levels of 1.0,2.0,and 10μg/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.

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 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]