全氟辛烷磺酰基化合物及全氟辛酸测试技术

为遏制全氟辛烷磺酰基化合物(PFOS)和全氟辛酸(PFOA)的全球性污染及对人类健康的危害,美、欧等国的有关部门及相关组织相继提出了禁止PFOS和PFOA生产及使用的规定.随着欧盟等对PFOS禁令的颁布和实施,PFOS和PFOA监测技术及分析方法研究倍受关注.然而,对于这些全氟化合物的定量测定,目前国际上尚无统一的标准...     

水产品中全氟辛酸和全氟辛烷磺酸检测技术 及污染现状

全氟辛酸(PFOA)和全氟辛烷磺酸(PFOS)是环境中广泛存在、较为典型的两种全氟化合物。针对水产品中PFOA和PFOS的检测技术和污染现状进行研究,进而研究其暴露途径、生物富集规律等内容,并基于此预测污染物环境分布、环境行为,以及相应地制定环境水和水产品质量安全标准,对于确保消费者食用安全具有重要意义。本文总结、分析了水产品中PFOA和PFOS的检测技术研究进展,及水环境和水产品中污染情况,对目前存在的问题及今后的研究方向进行了讨论和展望,以期为中国水产品中全氟化合物的监控和质量安全风险评估提供参考。     

全氟辛烷磺酸、全氟辛酸及其盐类检验技术的研究进展

全氟辛烷磺酸(PFOS)、全氟辛酸(PFOA)及其盐类物质具有生殖毒性、诱变毒性和发育毒性等多种毒性,也是目前最难降解的持久性有机污染物.全氟化合物独特的拒水拒油性,使其被广泛地应用于纺织、皮革、造纸等行业.PFOS和PFOA及其盐类物质通过食品包装材料,已经不知不觉进入我们的食品中,影响了食品安全,威胁着人们的身体健...     

采用高效液相色谱-电喷雾串联质谱法测定猪肉中的全氟化合物(PFOS、PFOA)

采用HPLC-ESI-MS/MS联用技术,建立了分析检测猪肉肌肉组织中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的方法.本方法以Waters sunfire C 18柱为液相分离柱,以乙腈-5mmol/L乙酸铵溶液梯度洗脱溶液,PFOS和PFOA在10min内即能达到良好分离,定性定量离子对分别为499.0/79....     

食品中全氟辛酸、全氟辛基磺酸的检测技术研究进展

全氟化合物(Perfluorinated compounds,PFCs)是一类含碳-氟键的高度稳定的极性有机化合物,全氟辛酸(Pentadecafluorooctanoic acid,PFOA)和全氟辛烷磺酸(Sperfluorooctanesulphonate,PFOS)是环境中广泛存在得两种典型全氟化合污染物,这两种典型的全氟化合物广泛应用于化工领域。此类全氟化合物因为具有持久的稳定性、生物积累性和多种毒性等,严重危害到了人类健康和其生存环境,多国政府纷纷颁布法令法规限制PFOA、PFOS的使用。因此食品基体中PFOA、PFOS的检测分析成为了当下分析科学研究的热点。本文首先对全氟化合物的结构、类型、极性等理化性质和全氟污染物的危害毒性进行概述,其次根据其化学性质以及参考国标等方法,梳理了国内外各种前处理方法,如：液液萃取、液固萃取、固相萃取、超声辅助萃取、QuEChERs等。其中QuEChERs方法结合多步净化方法能够最大程度降低食品中的基质效应。此外比较了气相色谱、液相色谱等方法在分离检测方面的优缺点,比较了已有文献中不同前处理方法和检测方法下的检出限、回收率、RSD等数据,结果发现UPLC-MS/MS法由于低检出限,方法稳定,检测快速,结果准确确等优点,仍为当下主流的检测手段。本文对于制定相应食品中全氟化合物质量安全标准,确保消费者食用安全具有重要意义,并总结了当下全氟化合物所遇检测的瓶颈,期望能为当下国内外全氟化合物污染防治和制定标准提供参考依据。     

纺织品全氟防水拒油易去污整理剂及其安全性

全氟烷基化合物作为防水、拒油和易去污多功能整理剂广泛用于纺织品、服装、皮革制品等的整理.文中通过全氟辛基磺酰化合物(PFOS)和全氟辛酸(PFOA)合成的防水、拒油、易去污整理剂的合成过程,以及表面化学基本原理阐明防水、拒油和易去污整理的机理.由于PFOS和PFOA的毒性,本世纪开始,欧盟和美国纷纷发布有关法令限制其生产和应用.     

制革行业中的全氟化合物及其检测

简单介绍了全氟化合物及其潜在的环境风险,概述了全氟化合物在制革工业中的应用,并对全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的分析检测方法进展进行了归纳和总结。     

鸡蛋中全氟化合物残留特征及其风险评估

为探究鸡蛋中全氟化合物(perfluorinated compounds,PFCs)的残留特征及其健康风险,采用离子对萃取与高效液相色谱质谱联用相结合的方法,对全国11个省(直辖市)产地鸡蛋中12种PFCs进行了分析,结果显示:全氟辛烷磺酸(perfluorooctane sulfonate,PFOS)与全氟辛酸(perfluorooctanoic acid,PFOA)是鸡蛋中主要残留物,东部沿海产鸡蛋中ΣPFCs高于内陆,北方产鸡蛋中PFOS含量较高,煮鸡蛋中ΣPFCs仅为生鸡蛋11%。PFOS、PFOA风险评估结果显示,鸡蛋中PFCs对人体不具即时危害。     

纺织品、皮革制品中全氟辛酸(PFOA)和全氟辛烷磺酸盐(PFOS)的测定方法初探

本文建立了一种PFOA和PFOS的高效液相—串联质谱(LC/MS/MS)测定方法。该方法简便快速,准确可靠,可应用于纺织品和皮革制品等工业产品中PFOA、PFOS的测定。     

皮革中全氟辛烷磺酸盐和全氟辛酸盐测定方法的优化

建立并优化了皮革样品中全氟辛烷磺酸盐(PFOS)和全氟辛酸盐(PFOA)的检测方法。在优化的提取温度和提取时间下,样品用甲基叔丁基醚–四丁基硫酸氢铵水溶液超声提取。提取液经浓缩、定容、过膜后,用超高效液相色谱–串联质谱(UPLC-MS/MS)检测。试验结果表明:在浓度范围0.5～20μg/L内PFOS和PFOA的标准曲线线性关系良好,方法的检测限均为0.25mg/kg,空白样品加标回收率分别在86%～96%和89%～103%之间,重复测量结果之间的相对标准偏差(RSD)小于10%。     

液相色谱串联质谱法测定纺织品中PFOS和PFOA

针对国际对纺织品中全氟辛磺酸(PFOS)和全氟辛酸(PFOA)的限量要求,采用ASE-300快速溶剂萃取仪提取样品中PFOS和PFOA,经浓缩、净化、过膜、定容后用液相色谱串联质谱法测定,外标法定量。采用选择离子检测进行阳性确证,建立纺织品中PFOS和PFOA的检测方法。该方法的最低检出限、线性范围和方法回收率对PFOS为1.0μg/kg、3.0~300μg/kg和82.35%~105.60%;对PFOA为0.5μg/kg、1.5~200μg/kg和85.17%~107.78%。     

基于液相色谱-串联质谱法的纺织品中痕量全氟化合物的测定

采用超声法提取纺织品中的全氟化合物。以C18为分析柱,甲醇-5 mmol/L乙酸铵为梯度洗脱淋洗液, 13 min内即可分离全氟己酸(PFHxA),全氟辛酸(PFOA),全氟壬酸(PFNA),全氟癸酸(PFDA),全氟十一酸(PFuDA),全氟十二酸(PFDoA), 全氟丁烷磺酸(PFBS),全氟己烷磺酸(PFHxS),全氟辛烷磺酸(PFOS),全氟癸烷磺酸(PFDS) 10种分析物。以313.1/268.9,412.9/368.9,462.9/418.9,512.7/468.9,562.7/518.9,612.8/568.9,298.8/99,399.2/99,498.8/99,599/99分别对PFHxA,PFOA,PFNA,PFDA,PFuDA,PFDoA,PFBS,PFHxS,PFOS,PFDS进行监控和定量分析。利用同位素内标法进行定量,线性范围和添加回收率分别为0.5～10 µg/m2、84.6%～111.8%,检出限为0.5 µg/m2,低于欧盟指定针对纺织品1 µg/m2 的限定。结果表明,本方法准确、快速,并成功用于20种纺织品实样的检测。     

Investigation into perfluoroalkyl substances (PFASs) in a cranberry bog: method development and sampling results

ABSTRACT

The contamination of groundwater and surface water from previous uses of perfluoroalkyl substances (PFASs), particularly products containing the contaminants perfluorooctane sulfonate (PFOS) and perfluorooctanoate (PFOA), has become a concern for drinking water and as a potential exposure route to the food supply. In 2016, the Food and Drug Administration (FDA) was asked to investigate a bog in Massachusetts where the surface water was believed to be contaminated with PFASs. As a result, a method was developed for the analysis of PFASs in cranberries, and water and fruit from the affected bog were evaluated. A QuEChERS method was developed and validated for PFOA, PFOS, and six additional shorter-chain PFASs. Method recoveries ranged from 60% to 115% for validation spikes performed at 10, 20 and 40 ng g^?1 and method detection limits ranged from 0.2 to 5.6 ng g^?1. Bog water samples were analysed using Environmental Protection Agency (EPA) method 537 for PFOA, PFOS and four additional short-chain PFASs. Surface water concentrations for PFOS ranged from 16 to 122 ng L^?1 and input water concentrations were 132 ng L^?1 and 206 ng L^?1. Of the eight water samples, seven had water concentrations that exceeded the EPA health advisory level for PFOS of 70 ng L^?1. Of the 42 cranberry samples analysed, none had detects of PFOA or PFOS above their method detection limits (0.4 and 0.5 ng g^?1, respectively), nor any of the other short-chain PFASs.     

柱上衍生气相色谱/质谱法测定纺织品中PFOS

全氟辛基磺酸(PFOS)很难通过常规方法从纺织品中分离、检出.采用超声-微波协同萃取仪提取样品中的PFOS,以四丁基氢氧化铵(TBAH)为衍生化试剂,与PFOS形成铵盐,再在柱上进行衍生化反应,形成PFOS丁酯,进而被气相色谱/质谱(GC/MS)联用仪检出.通过探索最佳衍生化反应条件,确立了柱上衍生GC/MS的检测方法,并对实际纺织样品中PFOS进行分离、检测,结果显示样品中的PFOS含量在0.59～11.27 mg/kg之间,能够满足国际法规对纺织品中PFOS的限量检测要求.     

Determinants of plasma PFOA and PFOS levels among 652 Danish men

Perfluorooctanoate (PFOA) and perfluorooctane sulfonate (PFOS) are used in a variety of industrial and consumer products and have been detected worldwide in human blood. The sources for human exposure are not well described, but dietary intake is suggested as an important source. In this study of 652 Danish men from the Diet, Cancer and Health cohort, we examined intake of 10 major dietary groups, tap water drinks, alcohol consumption, cooking method, geographical area, age, smoking status, and BMI as potential determinants of PFOA and PFOS plasma levels. Living in the Aarhus area was associated with higher PFOA and PFOS plasma levels compared with living in the Copenhagen area, and never smokers had higher levels than current smokers. Frying as compared with other cooking methods was a determinant of PFOA and PFOS levels. BMI and alcohol consumption were inversely associated with both compounds. Among the dietary groups, only intake of eggs was significantly positively associated with PFOS plasma levels. In future studies, PFOA and PFOS levels in air, dust and water samples should be measured to elucidate further the sources of exposure; exposure through diet needs to be studied in greater detail. Our finding of a higher body burden of PFOA and PFOS among never smokers also warrants further evaluation.     

Monitoring of perfluorinated compounds in edible fish from the Mediterranean Sea

Perfluorooctanoic acid (PFOA) and perfluorooctane sulphonate (PFOS) are environmental contaminants belonging to a chemical group known as perfluorinated compounds (PCFs). The United States Environmental Protection Agency (US EPA) considers both compounds to be carcinogenic. The goal of the present study was to evaluate the contamination levels of PFOS and PFOA in edible fish of the Mediterranean Sea. Twenty six fish muscles, 17 fish livers, five series of cephalopods (each composed of ten specimens) and thirteen series of bivalves (each composed of about 50 specimens) were used for the investigation. A fast sample treatment, followed by an LC–ESI–MS/MS method is described for the identification, and quantification of PFOA and PFOS in fish. The method was in-house-validated through the determination of precision, accuracy, specificity, calibration curve, decision limit (CCα), and detection capability (CCβ). The results showed PFOA and PFOS levels in fishes and molluscs lower than those reported for analogue matrices in different geographic areas. Therefore, our biomonitoring results did not show that the Mediterranean Sea had any particularly alarming pollution by PFCs, although it is located in a semi-closed basin with scarce water change. Nonetheless, a worrying element is that a few fish showed extremely high contamination by PFOA and PFOS. This finding needs further clarification in order to assess whether such unusual contamination is linked to “dot-like” pollutant release, which could explain the anomaly.     

Perfluorooctanesulfonate and related fluorochemicals in human blood from several countries

Perfluorooctanesulfonyl fluoride based compounds have been used in a wide variety of consumer products, such as carpets, upholstery, and textiles. These compounds degrade to perfluorooctanesulfonate (PFOS), a persistent metabolite that accumulates in tissues of humans and wildlife. Previous studies have reported the occurrence of PFOS, perfluorohexanesulfonate (PFHxS), perfluorooctanoate (PFOA), and perfluorooctanesulfonamide (PFOSA) in human sera collected from the United States. In this study, concentrations of PFOS, PFHxS, PFOA, and PFOSA were measured in 473 human blood/serum/plasma samples collected from the United States, Colombia, Brazil, Belgium, Italy, Poland, India, Malaysia, and Korea. Among the four perfluorochemicals measured, PFOS was the predominant compound found in blood. Concentrations of PFOS were the highest in the samples collected from the United States and Poland (>30 ng/mL); moderate in Korea, Belgium, Malaysia, Brazil, Italy, and Colombia (3 to 29 ng/mL); and lowest in India (<3 ng/mL). PFOA was the next most abundant perfluorochemical in blood samples, although the frequency of occurrence of this compound was relatively low. No age- or gender-related differences in the concentrations of PFOS and PFOA were found in serum samples. The degree of association between the concentrations of four perfluorochemicals varied, depending on the origin of the samples. These results suggested the existence of sources with varying levels and compositions of perfluorochemicals, and differences in exposure patterns to these chemicals, in various countries. In addition to the four target fluorochemicals measured, qualitative analysis of selected blood samples showed the presence of other perfluorochemicals such as perfluorodecanesulfonate (PFDS), perfluoroheptanoic acid (PFHpA), perfluorononanoic acid (PFNA), perfluorodecanoic acid (PFDA), perfluorododecanoic acid (PFDoA), and perfluoroundecanoic acid (PFUnDA) in serum samples, at concentrations approximately 5- to 10-fold lower than the concentration of PFOS. Further studies should focus on identifying sources and pathways of human exposure to perfluorochemicals.