摘要
新污染物可通过自然环境暴露迁移及生物积累的方式作用于人体,并引起毒副作用或慢性疾病而备受关注。由于新污染物覆盖目标物较为广泛,现有检测手段存在测试样本较为简单,测定方法较为繁杂的弊端。因此,本方法采用固相萃取法结合高效液相色谱-串联质谱联用技术,建立了猪五花肉中抗生素、全氟和多氟烷基物质、β-受体激动剂、内分泌干扰物、糖皮质激素和有机磷酸酯6个大类,共86种新污染物的检测方法。猪五花肉经80%乙腈水溶液(含0.5%甲酸)提取处理,氯化钠除水,采用CNW PPR Pro去磷脂小柱净化,40℃氮吹至尽干后,80%甲醇水复溶。使用CNW Athena UHPLC C18-AQ色谱柱(2.1 mm×100 mm,1.8μm)分离,5 mmol·L^(-1)甲酸铵-0.1%(V∶V)甲酸水溶液和乙腈为流动相,采用动态多反应监测(dMRM)采集并分析。在进行质谱分析过程中发现,甲酸与甲酸铵能够切实有效地提升目标物的离子化效率,并且显著改善目标物的响应峰形。PPR Pro与HLB和PSA这2种固相萃取填料比较发现,PPR Pro不仅能够保证较为稳定的绝对回收,同时能够有效抑制高脂肪基质引入的基质效应。本方法在0.5~50μg·L^(-1)线性范围内线性关系良好,决定系数(R^(2))在0.995~0.999范围内。3种不同质量浓度(0.25、2.50、25.00μg·kg^(-1))下平均回收率范围在65%~120%之间,相对标准偏差为1.0%~13.3%。该方法检出限范围为0.01~0.08μg·kg^(-1),定量限为0.04~0.25μg·kg^(-1)。本方法应用于9种猪五花肉,结果2份样本检出阳性,部分新污染物检出量较高。阳性样本中新污染物的暴露特征可能与环境污染及兽药残留相关,虽检出含量相对较低,但其长期暴露仍可能对环境和人类健康产生不利影响。该方法快速简便、灵敏度高、结果准确,适用于猪五花肉中6个大类新污染物精确定量,为新污染物对动物体危害的研究提供技术支持。
Emerging contaminants(ECs)of pollutants have attracted significant attention,as they can affect the h uman body through exposure,migration,and bioaccumulation in the natural environment,leading to toxic effects or chronic diseases.Given the wide range of EC types,the existing detection methods have limitations,particularly due to the high level of interfering substances in the samples,and the determination methods are complex.A method for 86 ECs in streaky pork was established for the determination by solid-phase extraction combined with high performance liquid chromatography-tandem mass spectrometry.The sample was extracted using 80%a queous acetonitrile solution(comprising 0.5%formic acid),and then the water and acetonitrile were separated by sodium chloride.After purification with the CNW PPR Pro phospholipid removal column,the extract was blown to dryness under nitrogen at 40℃and redissolved in 80%methanol.86 ECs were separated on CNW Athena U HPLC C18-AQ column(2.1 mm×100 mm,1.8μm)with 5 mmol·L^(-1) ammonium formate 0.1%formic acid a queous solution and acetonitrile as mobile phase.Dynamic multi-reaction monitoring mode was employed for d etermination.During the mass spectrometry analysis,it was found that formic acid and ammonium formate can e ffectively enhance the ionization efficiency of the target substance and significantly improve the response peak shape of the target substance.By comparing PPR Pro with HLB and PSA,it was found that PPR Pro can not only ensure a relatively stable absolute recovery rate but also effectively suppress the matrix effect introduced by high-fat-content pork.The method demonstrated linearity for 86 ECs in the concentration range of 0.5-50μg·L^(-1),with determination coefficients(R^(2))of 0.995-0.999.The recoveries of 86 ECs were 65%-120%at three different mass concentrations(0.25,2.50 and 25.00μg·kg^(-1)),with relative standard deviations in the range of 1.0%-13.3%.The limits of detection and quantitation of the method were 0.01-0.08μg·kg^(-1)and 0.04-0.25μg·kg^(-1),r espectively.The method was applied to 9 streaky pork samples,and 2 of them were detected positive.Notably,the detected levels of certain ECs in these positive samples were relatively high.The exposure characteristics of ECs in positive samples may be related to environmental pollution and veterinary drug residues.Although the detected content of ECs was relatively low,the long-term exposure to them may still have adverse effects on the e nvironment and human health.This method is rapid,simple,highly sensitive and accurate,making it suitable for the precise quantification of 6 major categories of ECs in streaky pork.It thus provides technical support for the research on the hazards of ECs to animal organisms.
作者
江晨舟
马海建
季瑞雪
张佳玉
赵晓祥
JIANG Chenzhou;MA Haijian;JI Ruixue;ZHANG Jiayu;ZHAO Xiaoxiang(ANPEL Laboratory Technologies(Shanghai)Inc.,Shanghai 201609,China;College of Environmental Science and Engineering,Dong Hua University,Shanghai 201620,China)
出处
《生态毒理学报》
北大核心
2025年第6期67-84,共18页
Asian Journal of Ecotoxicology
基金
上海市生态环境局资助项目(沪环科2021-10)。
关键词
抗生素
全氟和多氟烷基物质
有机磷酸酯
β-受体激动剂
内分泌干扰物
糖皮质激素
高效液相色谱-串联质谱法
猪五花肉
antibiotics
perfluoroalkyl and polyfluoroalkyl substances
organophosphate
β-agonists
endocrine d isruptor
glucocorticoids
high performance liquid chromatography-tandem mass spectrometry
streaky pork
