您所在位置： &
&nbsp&&nbsp&nbsp&&nbsp
用agilent 1290 infinity 液相色谱系统 uhplc 进行完整甘 ….pdf 8页
本文档一共被下载：
次 ,您可全文免费在线阅读后下载本文档。
下载提示
1.本站不保证该用户上传的文档完整性，不预览、不比对内容而直接下载产生的反悔问题本站不予受理。
2.该文档所得收入(下载+内容+预览三)归上传者、原创者。
3.登录后可充值，立即自动返金币，充值渠道很便利
需要金币：200 &&
用agilent 1290 infinity 液相色谱系统 uhplc 进行完整甘 …
你可能关注的文档：
··········
··········
--------------------------Page1------------------------------用Agilent1290Infinity液相色谱系统UHPLC进行完整甘油三酯的高分离度反相高效液相色谱分析应用报告食品，石化作者摘要迈克尔o伍德曼使用配置紫外/可见光（UV/VIS）二极管阵列检测器（DAD）的Agilent1290Infinity液安捷伦科技公司相色谱系统在无水反相梯度条件下，分析大豆油中的甘油三酯。使用Agilent1290Infinity桑特维利路液相色谱系统在不同长度、充填粒度、（）或（）0bar9000psi1200bar18,000psi威尔明顿,特拉华州19808压力下、内径为3.0mm和2.1mm的C18色谱柱上进行样品的色谱分离。本报告演示了美国异丙醇（IPA）或甲基叔丁基醚（MTBE）作为强溶剂和乙腈作为弱组分的混合流动相条件下，Agilent1290Infinity液相色谱系统能够采用高分离度长色谱柱。--------------------------Page2------------------------------前言对来自动物或植物的完整甘油三酯进行分析具有很强的实用价值，O包括加深对甘油三酯化学组成的理解、评估燃料潜热、了解生物系统的脂代谢行为。高效液相色谱（）成功分析这些组分的HCOOHPLC2基本条件包括：梯度洗脱及整体分离过程的低波长监测。甘油三*HCOO91215酯发色团相对较少，这有利于使用蒸发光散射检测器（ELSD）或HCOω2α质谱仪，以便于实现分离的其他目的。图1.典型的甘油三酯结构图在此应用的开发过程中，我们对来自大豆、玉米、米糠、红花、葡萄籽、橄榄及棕榈油的植物油进行了分析。由于大豆油在美国实广泛使用，且对生物燃料生产的意义不断增长，本应用的主要工作是最大限度地使大豆油甘油三酯的分离度符合标准要求。这些样品制备基本条件也适用于各种包括源自动物脂肪的样品。初始溶液的浓度为，异丙醇或甲醇甲基叔丁基醚体积10mg/mL/完整甘油三酯通常水溶性非常低，因此常采用常规色谱法进行分比为2:1，随后根据需要稀释到更低浓度。LC/DAD系统的进样离，该方法主要依靠极性功能团的差异分离样品，或非水分离模量为0.2-2uL。式的反相色谱法，它对于如链长或链不饱和度等碳性的微小差异LC方法详细说明有更好的选择性。液相色谱条件Agilent1290Infinity液相色谱系统二元泵G4220A,据珀金斯公布的资料[1]，在大豆油中发现的主要脂肪酸（甘油三Agilent1290Infinity液相色谱系统自动进样器G4226A酯的甘油骨干组成部分）是肉豆蔻（）、棕榈（）、油酸配切换阀的安捷伦柱温箱G:0配有10mm通径光纤流通池的Agilent1290Infinity液相色谱系统二极管阵列紫（）、亚油酸（）和亚麻酸（），也存在许多其他小脂肪18:118:218:3外/可见检测器G4212A酸。因为脂肪酸都是随机构造为甘油三脂，所以脂肪酸亚结构的色谱柱:（具体使用见各自的色谱图），广泛转换是可能存在的。由于脂肪酸之的主要差别是碳链长度AgilentZORBAXSB-C18RRHT3mm×150mm,1.8um600bar，部件号和双键数，所以甘油三酯的多样性主要呈现非极性有机结构的特AgilentZORBAXSB-C18RRHD,2.1mm×100mm,1.8um征。因此，反相色谱最适于此类应用。由于甘油三酯的水溶性极1200bar,部件号AgilentZORBAXSB-C18RRHD,2.1mm×150mm,1.8um差，您可以选择一个与水含量相关的较高的有机起始点，或如本1200bar,部件号报告，选择一个完全无水的分离环境。某些情况下，色谱柱要串联以增加长度和分离度柱温:20°C或30°C甘油三酯的典型结构如图1所示[2]。流动相：A=乙腈B=异丙醇(IPA)或甲基叔丁基醚(MTBE)（具体流动相见各自的在这个图中，从上到下，分别为棕榈酸（）、油酸（）、C16:0C18:1色谱图）亚麻酸（），显示了其链长和不饱和度。化学式为流速：具体流速见各自的色谱图a-C18:3梯度：基于与IPA相比，MTBE的洗脱强度高，梯度条件为20%至CHO。5598660%的异丙醇或10%至40%的MTBE。对于异丙醇梯度，梯度斜率一直维持在每柱容增加的有机相，为，相2.6%MTBE2.0%应地改变梯度时和流速。这是使用安捷伦方法转化器计算而确定的[3]。UV条件：监测210nm、220nm和230nm，带宽4nm，参考波长关闭2------------------------
正在加载中，请稍后...【图文】Agilent 1290 UHPLC方法转换过程_百度文库
两大类热门资源免费畅读
续费一年阅读会员，立省24元！
评价文档：
Agilent 1290 UHPLC方法转换过程
上传于|0|0|暂无简介
大小：299.82KB
登录百度文库，专享文档复制特权，财富值每天免费拿！
你可能喜欢Agilent1290液相色谱仪，进口液相色谱仪总代理_供应产品_郑州泽铭科技有限公司
郑州泽铭科技有限公司
血液酒精检测仪，全自动顶空进样器，氮氢空一体机发生器，白酒分析色谱仪，全自动血液酒精色谱仪，酒精检测仪
当前位置：
Agilent1290液相色谱仪，进口液相色谱仪总代理
240){this.width=240;}" onmouseover="SAlbum(this.src);" onmouseout="HAlbum();" onclick="PAlbum(this);" id="DIMG"/>
满足所有LC和LC/MS需求的更加卓绝的UHPLC系统 Agilent 1290 Infinity LC的设计是为了提供最高的分析速度、分离度和灵敏度。新的分析能力允许您采用任何类型的填料、任何规格的色谱柱，以及任何流动相和固定相。创新的技术元件将UHPLC和HPLC的应用提升到更高的性能水平...
产品详细介绍
无限的分析能力，结合高达1200 bar的超高压以及高达5 mL/min的高流速，最大程度地提升色谱性能、兼容性、灵活性和保障了投资回报&
&&& 由新型Agilent Jet We aver混合器的多层微流控技术所推动的新型1290 Infinity二元泵将主动阻尼与10 &L最低延迟体积相结合，可提供超高速的梯度洗脱，并能获得优异的紫外检测灵敏度
&&& 1290 Infinity二极管阵列检测器全新的光学设计&&包括Agilent 最大光强卡套式流通池&&使得UV灵敏度和基线稳定性达到了新水平，快速光谱采集的数据传输率高达160赫兹
&&& 1290 Infinity自动进样器的新一代高压单阀流路设计，无需更换样品环，为极小体积和大体积样品提供高精度进样
自动进样器相的新型1290 FlexCube，既可实现固定样品环进样模式下的超快速运行，又可通过对针座的自动反冲使交叉污染达到最低水平
&&&&1290 Infinity柱温箱的新型拉出式阀驱动器和用户可更换的阀头提高了使用性，并且为超高通量、多种方法和自动方法开发解决方案奠定了基础
&&&& 应用化学成分相同的新型ZORBAX快速分离高分辨（1.8 &m）液相色谱柱，能够方便，快捷和安全地将HPLC方法转移到UHPLC
&&& 新的实验室监控与诊断软件&&具有直观的诊断监控能力和预警功能，发现问题及时通知&&有助于对实验室进行管理，以获得最佳色谱质量
Agilent1290液相色谱仪&&&&& &Agilent1290 Infinity 液相色谱（LC）系统
&&& Agilent 1290 Infinity二元泵&&& 最宽范围的分析能力，具有完美的性能和灵活性&
&&& 新型1290 Infinity二元泵提供业界最宽范围的分析能力，具有极高的色谱性能和灵活性。最低延迟体积可以让您在窄径色谱柱上运行超快速梯度洗脱。主动阻尼与嵌入式固件的创新性泵设计相结合，显著降低了&泵波动&和相应的UV噪音。使用基于安捷伦的多层微流控技术的Jet Weaver混合器，进一步降低了背景噪音。新型陶瓷柱塞材料具有出色的热性能，即使在超高压下也能提供稳定可靠的性能。新的集成式高效脱气机和自动冲洗阀使得系统操作更为方便。&
&&& Agilent 1290 Infinity 自动进样器&&& 提供最高的进样精密度和最低的交叉污染的快速进样&
&&& 以新一代高压单阀流路设计为基础的自动进样器，无需更换定量管，即可为极小体积和大体积样品提供高精密度进样。一次进样，只需要进样体积的样品，将不会由于冲洗需要而将宝贵的样品浪费掉。计量装置的密封垫和针底座均采用惰性材料，并且减少了液压体积，可以使交叉污染降至最低。新的1290 Infinity FlexCube组件与自动进样器无缝结合，可获得完美的进样灵活性。FlexCube既可在超高速运行周期中的固定样品环进样，又能对自动进样器针座反冲，使交叉污染降至最低。&
&&& Agilent 1290 Infinity柱温箱&&适用的应用范围最广的柱温箱&
&&& Agilent 1290 Infinity 二极管阵列检测器&&以最高的采集速率达到最高的灵敏度&
&&& 1290 Infinity二极管阵列检测器（DAD）基于Agilent 最大光强卡套式流通池的光流波导进行了全新的光学设计。这种新的流通池技术利用全内反射的原理，极大地促进了光的传播，消除了流通池的分散效应导致的分辨率降低，从而使灵敏度达到了一个新的水平。几乎完全消除了任何可能带来不利影响的折光指数和热效应，大大减少了基线漂移，从而能够得到更可靠和更精确的色谱峰积分。1290 Infinity DAD以高达160 Hz的采集速率提供多波长和全谱检测，能够适应超高速液相色谱的分析速度
如果您觉得“Agilent1290液相色谱仪，进口液相色谱仪总代理”描述资料不够齐全，请联系我们获取详细资料。(联系时请告诉我从仪器交易网看到的，我们将给您最大优惠！)
本页链接：/com_zemingyiqi/sell/itemid-6412107.html
已经有741位访客查看了本页.
* 询价标题：
快捷提问：
请选择常用问题
我对贵公司的产品非常感兴趣，能否发一些详细资料给我参考？
请您发一份比较详细的产品规格说明，谢谢！
请问贵公司产品是否可以代理？代理条件是什么？
我公司有意购买此产品，可否提供此产品的报价单和最小起订量？
(不用打字 “快捷提问”帮您忙！)
* 主要内容：
*联系电话：
电子邮箱：
* 验证码：
公司名称：郑州泽铭科技有限公司
联系人：王保华
电话：0手机：传真：9邮件：地址：郑州市中原区238号凯旋门B座
供应产品新闻中心荣誉资质公司相册品牌展示&
&2017 郑州泽铭科技有限公司 版权所有
技术支持：&&&&访问量：199454
仪器交易网 设计制作，未经允许翻录必究.Copyright(C) 2014 , All rights reserved. 以上信息由企业自行提供，信息内容的真实性、准确性和合法性由相关企业负责，仪器交易网对此不承担任何保证责任。Per uorinated compounds (PFCs) are known for their high thermal and chemical stabilities and also for their water and oil repellent nature, which make them valuable for many industrial and commercial purposes. For example, polytetra fl uoroethylene (PTFE)-coated nonstick cookware, stain- and soil-resistant upholstery and textiles, and waterproof apparel (Gore-Tex). Some of these compounds, notably the per fl uoroalkyl acids (PFAAs), are used as surfactants, for example, per fl uorooctanoic acid (PFOA) and per fl uorooctanesulfonic acid (PFOS), during the production of fl uoropolymers, which in turn are used as resistant coatings on di ff erent surfaces. At the same time some of the PFAAs are degradation products of the aforementioned polymers. 1 As a result of their high chemical stability, the PFAAs tend to accumulate in the environment and living organisms. Many PFAAs are hepatotoxic 2 and carcinogenic. 3,4 It is therefore imperative to monitor their levels in the environment and food as well as the exposure of living organisms to PFAAs. There is currently no legislation in force limiting the levels of per fl uorinated organic substances such as PFOS or PFOA in food or feed within the European Union. In 2008, The Panel of Contaminants in the Food Chain (CONTAM) of the European Food Safety Agency (EFSA) performed a risk assessment of PFOS and PFOA and established a tolerable daily intake (TDI) of 150 ng/kg body weight for PFOS and 1500 ng/kg body weight for PFOA. 5 The occurrence of PFCs in food and dietary exposure was assessed in 2012 by EFSA. On the basis of the available data, exceedance of TDIs was found to be highly unlikely. 1 Numerous analytical methods have been developed for the quantitation of PFAAs in the environment and food with a focus on liquid chromatography coupled with tandem mass
spectrometry (LC-MS/MS) or gas chromatography mass spectrometry (GC-MS) methods. 6,7 GC-based methods require an 8 therefore, LC-based methods are simpler and usually preferred. Di ff erent sample preparation techniques have been used, such as pressurized liquid extraction 9,10 and solid-phase extraction (SPE) both o ffl ine and inline 11,12 with numerous solvents and additional sample concentrating methods. Although LC-MS/MS is one of the most selective techniques, the LC separation is still important to achieve accurate results, because electrospray ionization is prone components of a sample that are coeluted with the analyte may a ff ect the ionization process of compounds of interest. 13 Therefore, it would be ideal if the signal of an individual analyte would not be a ff ected by coeluting compound. PFAAs, both carboxylic and sulfonic, are strong acids and consequently are anionic at any realistic mobile phase pH. PFAAs are hydrophobic and lipophobic. The interaction of the per fl uoroalkyl groups with reversed phase stationary phases is not well understood, and the retention mechanism of these acids is unclear. They also undergo extensive aggregation even at very low concentration, 14,15 leading to micelle formation at about a concentration of 10 - 3 M. 16 In many cases separation of linear PFAAs with the same per fl uoroalkyl chain length has been problematic. 10,17 - 20 In particular, satisfactory liquid chromatographic separation of PFOS and per fl uorononanoic acid (PFNA) (both have C per uoroalkyl chains) has not always been achieved. For di ffi cult separations unusual stationary phases or mobile phase components have been used and in many cases successfully. Using fl uorinated stationary phases 21 - 23 or methylpiperidine as eluent modi fi er, 24 separation of PFNA and PFOS has been achieved successfully. In addition, a number of publications show the separation of PFNA and PFOS with C 18 stationary phases from di ff however, variations in eluent compositions and stationary phases make it di ffi cult to systematically analyze the retention mechanisms of those compounds on the basis of literature data. 25,26 From a mass spectrometric point of view PFOS displays some other inconvenient aspects when compared with per fl uorinated carboxylic acids of similar chain length. In the MS/MS regime it has a relatively low fragmentation yield and, as a consequence, a low S/N ratio. In the case of PFOS an MRM “ transition ” 499 → 499 (i.e., monitoring the non- fragmented parent) has been proposed. 27 However, the problem of accuracy remains, because in this case it has also been shown that certain steroidic bile acids present in fi sh samples have the same nominal m / z ratio of 499 with a similar fragmentation pattern and a retention time close to that of the PFOS and therefore may strongly a ff ect the peak area of PFOS. 22,27 The selection of eluent additives in LC-MS is limited by the volatility requirement. Fluorinated alcohols are volatile compounds of weak to medium acidity and are neutral in protonated form. These properties make them a potentially promising class of compounds to be used as weak acids for preparing bu ff ers of pH value above 7 for use in LC-MS. 1,1,1,3,3,3-Hexa fl uoro-2-propanol (HFIP, p K a = 9.3) 24 has been used as an additive to the LC mobile phase in several studies. 28 - 35 The suitability of fl uoroalcohols, HFIP and 1,1,1,3,3,3-hexa fl uoro-2-methyl-2-propanol (HFTB, p K a = 9.6) 36 , as bu ff er additives at concentration levels from 1 to 10 mM has been studied, and application for separation of antibiotics - fl uoroquinolones and sulfonamides is demonstrated. 37,38 It turned out that mobile phases with per fl uorinated alcohols provide retention mechanisms that di ff er from the ones traditionally observed with regular eluent modi fi ers for C 18 stationary phases. 38 Alternatively, a promising group of stationary phases that have been successfully applied in pharmaceutical and drug analysis are fl uorinated (penta fl uorophenyl and penta fl uor- ophenylpropyl) stationary phases. 39 - 41 Fluorinated stationary phases are associated with various interaction mechanisms improving retention and chromatographic resolution. Most similar to common stationary phases are per fl uorinated alkyl chains, for example, C 8 F 17 , used for their alternative retention in several applications for separating polar molecules, 42,43 especially halogenated analytes, 44 - 47 but also for aromatic polycyclic hydrocarbons due to the interactions between π electrons of analytes and C - F dipole of the stationary phase. 46,48 The performance of fl uorinated columns has improved in recent years with respect to their pH stability and column lifetime. Additionally, stationary phase bleeding is reduced, allowing the use of these stationary phases also in MS applications. The retention of all analytes has been reported to be overall lower on the fl uorinated stationary phase than on C 18 . 47 Therefore, the retention of PFCs using a fl uorinated stationary phase and fl uoroalcohols with a regular C 18 stationary phase is of interest. The focus of this work is the LC-ESI-MS analysis of PFOA, PFNA, and PFOS in raw fi sh samples using a di ff erent approach for chromatographic separation and signal improvement: replacement of common eluent bu ff ers (ammonium acetate) with a poly fl uorinated alcohol - ammonia bu ff er. 34,36 Separations of structurally similar per uorinated compounds on C 18 stationary phases have been problematic in several previous studies. 10,17 - 20 In this study the retentions of the analytes on the C 18 stationary phase were similar using 0.1% formic acid (pH 2.6) and MeCN in eluent, and separation between the three analytes was not achieved. Asymmetrical and wide peaks eluted with 82% of MeCN. However, the previous studies indicate separation of PFOA, PFNA, and PFOS using per fl uorinated stationary phase, 21 and retention of fl uorinated compounds is enhanced on fl uorous stationary phases. 47 The separation of PFOA, PFNA, and PFOS was studied using an alkyl per fl uorinated stationary phase. Fluorinated analytes ’ retention on the fl uorinated stationary phase is mainly in fl uenced by the amount on fl uorine atoms in the analyte molecule. 47 The number of fl uorine atoms in PFOA molecule is 15; on the other hand, PFNA and PFOS have equally similar 17 fl uorine atoms in the molecule. To achieve advanced separation for analytes, a fl uorinated stationary phase was tested in this work. An Epic FO LB (150 mm × 3.0 mm, 3 μ m) column meant for separating fl uorinated compounds demonstrated signi fi cant column bleed and contaminated the source very quickly. In addition, separation of PFNA and PFOS was not observed (Figure 1). Because the Epic FO LB column showed inadequate separation of compounds and signi fi cant source contamination was observed, and in addition the column maximum pH range was 8, further attempts were made with a C 18 stationary phase using 5 mM ammonium acetate at higher pH values (pH 9 and 10) as a component of eluent. Therefore, the change in eluent pH was made and 5 mM ammonium acetate (pH 10) was used for elution. Increased eluent pH with the C 18 column (YMC Triart C18) led to better peak shape on the chromatogram, but the analysis of PFNA and PFOS was still problematic due to the low S/N ratio (Figure 2). To enhance separation of analytes on the C 18 stationary phase, alternative eluent components were used: 5 mM HFIP and 5 mM HFTB at the same pH as ammonium acetate (pH 10). The resolution, assessed as the R s values, of the analyzed compounds using 5 mM HFTB was slightly better at pH 10 (Figure 3) compared to ammonium acetate and HFIP bu ff er. However, the used MeOH content at the retention time of the
with HFTB the MeOH content was in the range of 62 - 63%, and with ammonium acetate the content was in the range of 83 - 84%. Thus, the use of poly fl uorinated alcohols can enhance the separation of fl uorinated compounds, leading to alternative selectivity due to the fl uoroalcohol competition over the C 18 stationary phase surface. Fluoroalcohols tend to “ stick ” on the C 18 surface, covering the surface with a fl uorous layer and shifting the stationary phase properties nearer to a fl uorinated stationary phase. This enhances the separation of PFAAs. On the other hand, the stationary phase has a negative charge on its surface due to the negatively charged HFTB molecules at pH 10. PFOS and PFNA are deprotonated at pH 10, and the two anions are rather similar by their size and charge distribution. As a di ff erence, however, the negative charge on the PFOS anion is more e ffi ciently delocalized over the larger SO 3 - moiety than is possible in the PFNA anion ’ s smaller CO - moiety. This leads to more e cient solvation of the carboxylate center by water molecules than of the sulfonate center. 52,53 The negative charge localization in the PFNA anion leads to two consequences: (1) it is better solvated by the polar mobile phase and is thus less forced out of the mobile phase and (2) possibly the repulsion between the partially negatively charged stationary phase surface and the PFNA anion is stronger than the repulsion between the stationary phase and the PFOS anion, leading to decreased retention of the PFNA anion on the stationary phase, compared to the PFOS anion. This di ff erence between the anions of PFNA and PFOS is small, however, and therefore their retention times are still very similar. In addition, their retention can be decreased due to the competition of bu ff er additive and analytes for the stationary phase surface. Even though the MeOH content of eluent was lower at the analyte ’ s retention time using 5 mM HFTB as additive, signi fi cant signal improvement (by 2 - 8 times in peak area) was observed when using HFTB as eluent component when compared to the ammonium acetate at low analyte concentrations (10 ng/mL) (Figure 4). Method Validation. For the calibration graph solutions, appropriate dilutions from working standard in the concentration range of 1 - 600 ng/mL ( n = 14) for PFOA, PFNA, and PFOS were made in MeOH. The overall range was divided into three independent narrower calibration ranges: 1 - 15 ng/mL ( n = 5), 15 - 110 ng/mL ( n = 6), and 110 - 600 ng/mL ( n = 5). The calibration graphs showed adequate linearity in the narrower concentration ranges ( r 2 ≥ 0.9902). An unweighted linear regression analysis of representative calibration curves resulted in slopes of 17.3 (PFOA), 18.2 (PFNA), and 4.0 (PFOS) in the lower concentration region and of 13.5 (PFOA), 14.3 (PFNA), and 2.5 (PFOS) in the higher concentration region. The intercepts of the calibration curves were taken into account for PFOA (50.6), PFNA (5.9), and PFOS (1.1) in the lower concentration range and for PFOA (499.6), PFNA (600.6), and for PFOS (186) in the higher concentration range. Spiking experiments for method validation were performed so that concentrations in samples corresponded to 1, 10, and 100 μ g/kg. Samples were spiked before the second homogenization step with 1 mL of spiking solutions with di ff erent concentrations (7.5, 75, and 750 ng/mL) and mixed thoroughly. After homogenization, 14 mL of acetonitrile was added and the procedure was continued as described above. The average process e ffi ciency (including sample preparation recovery and matrix e ff ect) for the studied compounds was in the range of 99 - 116% and exceptionally 115 - 143% for PFOS in the low concentration range. The matrix e ff ects were evaluated using post extraction spiking (salmon extract) and a signal-enhancing e ff ect was determined: up to 120 - 141% for PFOA, 136 - 178% for PFNA, and 132 - 189% for PFOS. The recovery rates were estimated over the calibration range and were in the ranges of 88 - 133% for PFOA, 85 - 108% for PFNA, and 70 - 98% for PFOS. The LOQ and LOD were estimated (as 10 and 3.3 times the standard deviation, respectively) from six replicate analyses of unspiked and pre-extraction spiked salmon samples (Figure 5). Method accuracy and precision were estimated from the spiked salmon samples at the three concentrations of 1, 10, and 100 μ g/kg. Accuracy was estimated as the closeness of mean test results obtained by the method to the true concentration value of the analyte and ranged from 2 to 9% for all analytes at high, medium, and low concentrations. Precision was estimated as coe ffi cient of variation (CV) at three concentration levels and is presented in Table 2. It has been stressed that due to the Te on tubing of chromatographic systems a signi fi cant contamination of PFAAs might occur and therefore a trapping column has been used, which catches PFAAs originating from tubing. 49 In this work a trapping column was not used and blank injections were monitored constantly to determine the extent of contamination, and the average area of blank injection peaks within sequences was subtracted from standard and sample chromatograms. Method Application to Fish Samples. For practical application this method was transferred to a di ff erent LC-MS system, validated for the Estonian Health Board Tartu laboratory, and tested on number of samples available in Estonia. Of the 20 analyzed samples, 7 originated from the Baltic sea, 3 from Norway, 4 from fresh water fi sh farms, and 6 from fresh waters of Estonia. All of the samples were analyzed twice on two separate days. The content of PFOA remained below the LOD in all samples. PFNA was found to be present at low concentrations in seven samples, and in two cases the content exceeded the LOQ. PFOS was found to be present in six samples, and the concentration exceeded the LOQ in three samples (see Table 1). Due to the low salinity of the Baltic Sea many species that usually live in fresh water can also be found in marine water. The obtained results for the fi sh samples from the Baltic Sea are comparable with previous studies. 54 PFC bioaccumulation in organisms has increased signi fi cantly, and the research conducted in the Baltic Sea area has focused on analyzing fi sh, predatory mammals, and birds. The concentrations of PFAAs is signi fi cantly higher in mammals and birds. 55,56 PFOS is one of the core indicators for the Baltic Marine Environment Protetction Commission (HELCOM), and its levels in fi sh livers and muscle have been analyzed overa long period of time. Concentrations of PFOS have been dependent on the species of fi sh and catching area, showing elevated levels of PFOS from parts of the Baltic Sea where industrial activity is more intense. 56 In 2010 Hradkova et al. analyzed the contents of PFOA, PFOS, and per fl uorooctane sulfonamide in canned fi sh products available in Czech Republic and found that most contaminated samples originated from the Baltic Sea. 58 Their study showed also that concentrations of PFOS and PFOA vary to a great extent despite the similari one particular type of sample originating from the same country (sardines in oil) contained PFOS from below the LOQ (0.3 μ g/kg) to 12.8 μ g/kg and PFOA from below the LOQ (0.2 μ g/ kg) to 5.1 μ g/kg of PFOA, which is supposedly related to the catch site. 57 Similar variations of PFOS and PFOA contents were also shown by Lacina et al. in the case of canned cod liver originating from the Baltic Sea. 49 In the current work, similarly to previous studies, PFOS was found to be in higher content than other PFAAs. However, the content of PFOS was higher in fi sh samples originating from the Baltic Sea than compared with fresh water. Obtained results are diverse compared with previous studies. 54,59 This can be explained by a lower population density and the lack of intense industrial activity in Estonia compared with Germany and Sweden. QuEChERS-type sample preparation with cleanup has proven to be a reliable method on many occasions when di ff erent types of contaminants such as pesticides, acrylamide, and mycotoxins have been analyzed in food samples. 60 - 62 Sample preparation is fast and simple and removes unwanted sample components such as fats, proteins, and starch from the extract. Conclusions. This work describes an alternative method for LC-MS/MS analysis of per fl uorinated compounds in fi sh using a novel eluent additive. The method uses simpli fi ed sample treatment but still provides su ffi cient LC selectivity and enhanced signal intensities for analytes. An important factor for achieving this is applying poly fl uorinated alcohol (HFTB) in the chromatographic separation. Brief monitoring of Estonian fresh and marine water fi sh was carried out, and the content of PFAAs was low. E-mail: karin.. Fax: +372 737 5264. Phone: +372 566 675 04. This work was supported by Grant 8572 from the Estonian Science foundation, by Institutional Funding IUT20-14 (TLOKT14014I) from the Estonian Ministry of Education and Science, and by the Estonian Ministry of Agriculture (under the state project “ Agricultural applied research and development in 2009 - 2014 ” ).Join ResearchGate to access over 30 million figures and 100+ million publications – all in one place.Copy referenceCopy captionEmbed figurePublished in
Full-text available &
Article & May 2014
& Journal of Agricultural and Food Chemistry
+3 more authors...
ABSTRACT: Perfluorinated compounds (PFCs) are a group of organofluorine, aliphatic hydrocarbons, which all or almost all hydrogen atoms are replaced with fluorine. They have a wide range of industrial and consumer applications such as stain, paints, hydraulic fluids, firefighting foams, production of fluoropolimers, cosmetics, insecticide formulations, textile treatments, surface coatings for carpets and furniture, cookware and water- and oil- resistant coatings for food contact materials. PFCs are extremely resistant towards thermal, chemical and biological degradation processes. There is now no evidence for their degradability and they decomposed only at very high temperatures, and specially prepared furnaces.
PFCs tend to accumulate in food chain and animal and human target organs. They have been detected globally as pollutants in water, plants, sediments, foodstuffs, and in animals such as fish, birds, mammals, as well as in human breast milk and blood.
Currently, human are on the increased risk as PFCs are resistant to hydrolysis, photolysis, microbial degradation or metabolism. The two most frequently studied PFCs are perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS), generally considered reference substances. Their estimated elimination half-life is about 3.8 years for PFOA and 5.4 years for PFOS. It is fully justified, because all of the perfluorooctanesulfonyl fluorine (POSF)-based compounds biologically break down or become metabolised to PFOS. PFOA, in addition to its production and use as a surfactant, is also formed as a degradation product of several fluoropolymers and fluorotelomer alcohol. There is currently no legislation for perfluorinated organic substances such as PFOA and PFOS in food or feed within the EU.
There is a number of pathways by which PFCs contamination of humans can take place including diet, food contact materials, non-food personal items, and indoor and outdoor air. Perfluorinated compounds bind to serum albumin and other cytosolic proteins and accumulate mainly in liver and kidney. An important number of studies show that PFCs cause a wide range of negative effects, including hepatic diseases, reproductive toxicity, immunotoxicity, and neurotoxicity. An in vitro and in vivo studies have started to investigate the molecular mechanisms by which PFOA and PFOS exert their adverse effects. However, the specific mechanisms related to these adverse effects is far from being clear.
This chapter summarizes the recent information on the occurrence, exposure and health effects caused by PFOA and PFOS – the two main representatives of the perfluorinated compounds.Chapter · Feb 2016 · Environmental Toxicology and ChemistryABSTRACT: To address the health and environmental concerns associated with perfluorocarboxylic acids, the assessment of cytotoxicity and bioaccumulation of perfluorocarboxylic acids is essential. This study investigated the effect of perfluorocarboxylic acids having various chain lengths on mouse melanoma B16 cells. The extent of cytotoxicity of perfluorohexanoic acid (C6), perfluoroheptanoic acid (C7), perfluorooctanoic acid (C8), perfluorononanoic acid (C9) and perfluorodecanoic acid (C10) within a concentration range of 0.25–1600 μg/ml was determined. Based on results, the viability of cells was 90% or higher in the presence of C6, C7, C8 at a concentration of up to 200 μg/ml, indicating that B16 cells are safe in the presence of C6, C7 and C8. On the other hand, moderate cytotoxicity was observed with C9 or C10, even at a relatively low concentration of 25 μg/ml. When cells were incubated in the presence of the same concentration (100 or 200 μg/ml) of perfluorocarboxylic acids, the number of live cells decreased as the perfluoroalkyl chain length increased suggesting that long-chained perfluorocarboxylic acids are more cytotoxic than short-chained perfluorocarboxylic acids. The correlation between cellular uptake and perfluoroalkyl chain length was also investigated. The presence of C6 in the cells was not detected probably because of poor uptake. On the other hand, the presence of C7–C10 in the cells was confirmed and quantified by LC ESI MS. Results showed that cellular uptake of long-chained perfluorocarboxylic acids were significantly higher than short-chained perfluorocarboxylic acids.Article · May 2016 ABSTRACT: Perfluoroalkyl substances (PFAS) have recently received increased research attention, particularly concerning aquatic organisms and in regions of exposure to Aqueous Film Forming Foams (AFFFs). Air Force bases historically applied AFFFs in the interest of fire training exercises and have since expressed concern for PFAS contamination in biota from water bodies surrounding former fire training areas. We monitored six PFASs, including perfluorooctane sulfonate (PFOS), in aquatic species from eight bayou locations at Barksdale Air Force Base in Bossier City, Louisiana over the course of one year. Our focus was to evaluate temporal and spatial variability in PFAS concentrations from historic use of AFFF. PFOS concentrations in fish tissues peaked in early summer, and also increased significantly downstream of former fire training areas. Benthic organisms had lower PFOS concentrations than pelagic species, contrary to previous literature observations. Bioconcentration factors varied with time, however were reduced as compared to previously reported literature values. Here we report the highest concentration of PFOS in whole fish (9,349 ng/g dw), with 15% of samples exceeding what we believe to be the maximum whole fish concentration reported to date of 1,500 ng/g ww. Future studies to measure PFAS in larger fish and tissue specific partitioning data to compare to the current whole fish values are ongoing. The high concentrations observed presently could have effects for higher trophic level organisms in this system or potential risk to humans consuming contaminated fish. This article is protected by copyright. All rights reserved.Article · Dec 2016 +1 more author...