Compounds In Fish Samples Research Articles

Determination of 19 chlorophenols in fish by QuEChERS-gas chromatography-mass spectrometry

大量含氯农药、次氯酸消毒水以及水产品杀虫剂和杀菌剂的广泛使用,使鱼类容易受到氯酚类化合物的污染,因而建立鱼肉中氯酚类化合物的检测方法十分重要。建立了QuEChERS结合气相色谱-质谱法同时检测鱼肉中19种氯酚类化合物的分析方法。19种氯酚类化合物选用DB-5MS毛细管色谱柱(30 m×0.25 mm×0.25 μm),载气流速1 mL/min进行分离,可以得到很好的峰形。前处理采用改良的QuEChERS方法,通过对提取剂的种类和剂量、净化剂的种类和剂量,以及衍生条件中的衍生温度、衍生时间和衍生剂用量等进行优化,确定最优的前处理方法。选择10 mL乙酸乙酯作为提取剂,500 mg的C18作为净化剂,加入3 g氯化钠和5 g无水硫酸镁,过0.22 μm的有机滤膜,加入50 μL的硅烷化衍生剂在45 ℃条件下衍生30 min,用EI源测定,选择离子监测模式,以外标法定量。19种氯酚类化合物在0.4~10 μg/L范围内具有良好的线性关系,相关系数R2大于0.998,方法定量限为0.04~0.16 μg/kg。空白基质不同加标水平的回收率为70.6%~115.0%,相对标准偏差为2.6%~10.5%。将建立的方法应用于实际样品的检测分析,结果显示,各种鱼肉中均有不同程度的氯酚类化合物检出,其中,黄花鱼检出的氯酚类化合物总量最大,为8.74 μg/kg;其次为鲫鱼7.59 μg/kg;米鱼的检出量最少,为1.59 μg/kg。所建立的方法简化了样品的前处理步骤,操作简单,方法灵敏度高、重复性好,可满足鱼肉中19种氯酚类化合物的高通量检测要求,能显著提高氯酚类化合物的检测效率。

Occurrence of benzotriazole UV stabilizers in coastal fishes

Chemicals added in personal care products are of emerging concern because their fate and their effect on the environment is not completely known. Benzotriazole UV stabilizers (BUVSs) are compounds used in different cosmetic products, which may reach the marine environment through marine discharge from treated waters or directly from bathing areas. Once released into the aquatic ecosystem, BUVSs can be bioaccumulated by aquatic organisms. To identify the human exposure risk, it is important to have suitable analytical methods to determine the presence of BUVSs in these organisms. Because of the complexity of such a biological matrix, selective extraction and detection techniques are required to isolate and quantify these kinds of pollutants at trace levels. In the present work, we optimized a method based on microwave-assisted extraction combined with ultra-high performance liquid chromatography and mass spectrometry detection to determine six benzotriazole compounds in fish samples. The absolute extraction yields provided by the proposed method were higher than 40% for most compounds, with intra-day and inter-day relative standard deviations ranging from 0.27 to 6.06 and 1.12–21.3%, respectively. The limits of quantification were in the range of 1.13–9.66 ng g−1 (dry weight). The method was applied to the study of three species of fish (Boops boops, Sphyraena viridensis, Sphoeroides marmoratus) that were collected close to three marine outfalls of treated waters on the Gran Canaria Island (Spain) for two years. Four of the six studied compounds, UV-326, UV-328, UV-329 and UV-360, were found with concentrations ranging from 1.34 ng g−1 to 45.6 ng g−1 (dry weight).

Analysis of Halogenated Compounds in Fish Samples

The paper reports investigation on the presence of 13 halogenated compounds (six chlorinated compounds, nd-like PCBs and seven brominated compounds, polybrominated diphenyl ethers (PBDEs)), in five marine species which are part on Albanian consumer diet. The samples were extracted with ethyl acetate and treated with sulfuric acid. Extract was analyzed simultaneously using gas chromatography tandem mass spectrometry. Presence of PCBs was confirmed at1.4 percent of the samples. The most dominated congener found to be present were PCB 153 and PCB 138. Form the brominated compounds 2,2′,4,4′-tetra-bromodiphenyl ether was the only detected compound in 3 samples.

Analysis of Halogenated Compounds in Fish Samples

The paper reports investigation on the presence of 13 halogenated compounds (six chlorinated compounds, nd-like PCBs and seven brominated compounds, polybrominated diphenyl ethers (PBDEs)), in five marine species which are part on Albanian consumer diet. The samples were extracted with ethyl acetate and treated with sulfuric acid. Extract was analyzed simultaneously using gas chromatography tandem mass spectrometry. Presence of PCBs was confirmed at1.4 percent of the samples. The most dominated congener found to be present were PCB 153 and PCB 138. Form the brominated compounds 2,2?,4,4?-tetra-bromodiphenyl ether was the only detected compound in 3 samples.

Rapid Sample Preparation Method with High Lipid Removal Efficiency for Determination of Sulphuric Acid Stable Organic Compounds in Fish Samples

A rapid and low-cost sample preparation method modifying the so-called QuEChERS (quick, easy, cheap, effective, rugged and safe) method was developed for the determination of H2SO4 stable organic compounds in fish samples. The method involves acetonitrile salting-out extraction and a novel clean-up procedure combining the pH-tuned dispersive liquid–liquid microextraction (DLLME) with conc. H2SO4 digestion. The H2SO4 treatment is carried out by a simple operation in contrast to laborious and time-consuming procedures reported in the literature. The method was developed, optimised and validated using selected polybrominated diphenyl ethers (PBDEs) as representatives of H2SO4 stable compounds. For instrumental analysis of sample extracts, thermal desorption–gas chromatography–triple quadrupole tandem mass spectrometry (TD–GC–QqQ-MS/MS) was used. The proposed sample preparation method provides better co-extractives removal efficiency as compared to the original QuEChERS method and, unlike the QuEChERS dispersive solid-phase extraction (dSPE), allows complete removal of fatty acids. The sample preparation is low-cost due to the employment of small amounts of low-cost chemicals (no need of expensive sorbents), and it does not require special instrumentation. The whole analytical method showed satisfactory performance (linearity, recovery, repeatability, accuracy, limits of the method), and its applicability was confirmed by determination of PBDEs in samples of four fish species with variable lipid content in the range of 0.7–19%. The obtained recoveries for six PBDEs in the NIST standard reference material SRM 1946 were in the range of 81–95%, and relative standard deviations were in the range of 3–13%.

Tuneable surface enhanced Raman spectroscopy hyphenated to chemically derivatized thin-layer chromatography plates for screening histamine in fish.

Reliable screening of histamine in fish was of urgent importance for food safety. This work presented a highly selective surface enhanced Raman spectroscopy (SERS) method mediated by thin-layer chromatography (TLC), which was tailored for identification and quantitation of histamine. Following separation and derivatization with fluram, plates were assayed with SERS, jointly using silver nanoparticle and NaCl. The latter dramatically suppressed the masking effect caused by excessive fluram throughout the plate, thus offering clear baseline and intensive Raman fingerprints specific to the analyte. Under optimized conditions, the usability of this method was validated by identifying the structural fingerprints of both targeted and unknown compounds in fish samples. Meanwhile, the quantitative results of this method agreed with those by an HPLC method officially suggested by EU for histamine determination. Showing remarkable cost-efficiency and user-friendliness, this facile TLC-SERS method was indeed screening-oriented and may be more attractive to controlling laboratories of limited resource.

Food Processing Effect on the Residue Levels of Organochlorine Compounds In Fishes

A study was conducted to screen certain pesticide residues such as Organochlorine compounds in fish samples and to assess the effect of food processing methods on degradation of residue levels in both natural and spiked samples. Fish samples were collected from local areas of Hyderabad, Telangana, India and subjected to various food processing such as boiling and broiling and samples were analyzed by using Gas Chromatography- Electron Capture Detector by employing QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method for sample extraction and cleanup process. The final mean residual levels and their degradation percentage was also calculated with respective treatments. Heat processing methods proved to be highly effective on degradation of some Organochlorine compounds in both natural and spiked samples of fishes. Both the treatments i.e. boiling and broiling were statistically nonsignificant on degradation of respective pesticides in both natural and spiked samples of fishes.

Speciation analysis of mercury in natural water and fish samples by using capillary electrophoresis–inductively coupled plasma mass spectrometry

A environment-friendly microwave-assisted extraction used to extract trace mercury compounds from fish samples, and a ultra-sensitive method for the analysis of Hg(II), methylmercury (MeHg) and ethylmercury (EtHg) by using capillary electrophoresis–inductively coupled plasma mass spectrometry (CE–ICP–MS) were described in this study. The extraction method is environment-friendly, simple, effective, and can be used to extract trace mercury compounds in fish samples with a satisfied recovery within several minutes. The CE–ICP–MS analytical method has a detection limit as lower as 0.021–0.032ng Hg/mL for MeHg, EtHg and Hg(II), and can be used to determined ultratrace MeHg, EtHg and Hg(II) in natural water and fish samples directly without any preconcentration. With the help of the above methods, we have successfully determined MeHg, EtHg and Hg(II) in dried fish (Tapertail anchovy) muscle and natural water within 25min with a RSD (relative standard deviation, n=6) <5% and a recovery of 94–103%. Our results showed that dried muscle of T. anchovy contained only one species of mercury, MeHg, indicating that MeHg is easier to be accumulated by aquatic organisms.

Gas chromatography–ion trap tandem mass spectrometry method for the analysis of methoxylated polybrominated diphenyl ethers in fish

Gas chromatography coupled to ion trap tandem mass spectrometry (GC–ITMS-MS) is proposed for the analysis of methoxylated polybrominated diphenyl ethers (MeO-PBDEs) in fish and shellfish. MS–MS operating parameters related to the isolation and fragmentation of the precursor ions were optimized to achieve maximum sensitivity and selectivity. This new method allows the determination of both MeO-PBDEs and PBDEs in a single run. Low limits of detection (0.4–2.5 pg injected) and high precision (RSD < 13%) were achieved. A sample treatment based on a selective pressurized liquid extraction (PLE) using Florisil as fat retainer was applied for the analysis of these compounds in fish samples. Method limits of quantification ranged from 0.11 to 0.95 ng g −1 lipid weight for MeO-PBDEs and between 0.18 and 0.50 ng g −1 lipid weight for PBDEs. In addition, good repeatability of the whole method was achieved (RSD < 15%). The suitability of the method was evaluated by analyzing a certified reference material (SRM 1945, whale blubber) with satisfactory results. The developed method was applied to the simultaneous analysis of MeO-PBDEs and PBDEs in fish and shellfish samples from the Mediterranean Sea.

Biomonitoring as assessment of human exposure to heavy metals. Speciation of Hg in fish food and impact on human health

A biomonitoring method has been developed for determination of both inorganic and organic Hg in fresh and canned fish and also in blood based on ICP–MS coupled with high performance liquid chromatography (HPLC). In this way, the species of Hg which are present in organic samples like fish food can be determined. The speciation was developed to determine the methyl mercury content and, concomitantly, the atomic absorption spectroscopy method was used to determine the total mercury content in fish food. The present study reports the concentrations of total mercury and its speciation in fresh and canned fish food and these amounts have been found to be significantly higher in predatory species of fish while the most abundant species was methyl mercury. Moreover, some correlations have been performed between biomonitoring results and determination of mercury compounds in fish samples purchased from a local market in order to evaluate the speciation of Hg in fish food.

Gas chromatography retention data of environmentally relevant polybrominated compounds

Polybrominated organic compounds are ubiquitous throughout the environment. This generic term comprises several classes of brominated flame retardants (e.g., polybrominated diphenyl ethers, polybrominated biphenyls, hexabromocyclododecane, dibromopropyltribromophenyl ether, 1,2-bis(2,4,6-tribromophenoxy)ethane) as well as a range of marine halogenated natural products (HNPs). Here we present gas chromatography retention times and elution orders (on DB-5) of 122 polybrominated compounds that may be found in food and environmental samples. Organobromine compounds in fish samples determined with gas chromatography interfaced to electron-capture negative ion mass spectrometry (GC/ECNI-MS) are discussed. The environmental relevance and important mass spectrometric features of the compounds are described as well. Our database aims to support the closer inspection and identification of peaks in gas chromatograms and to initiate dedicated screening for less frequently studied organobromines in samples.

Speciation of organotin compounds in fish samples

The optimization of extraction and determination of organotin compounds in fish samples using aqueous ethylation, gas chromatographic separation and on-line quartz furnace atomic absorption spectrometric detection (Eth–GC–AAS) has been studied. Digestion with 0.5 mol l–1 methanolic HCl or 0.5 mol l–1 methanolic acetic acid assisted by sonication or microwave agitation is proposed. Limits of detection of Sn of 2–4 ng g–1(fresh mass) for methyltin and butyltin compounds could be achieved. The analysis of fresh samples is mandatory to avoid any possible losses of organotin species during drying procedures.

Determination of volatile organic compounds in fish samples by vacuum distillation and fused silica capillary gas chromatography/mass spectrometry.

Determination of volatile organic compounds in fish samples by vacuum distillation and fused silica capillary gas chromatography/mass spectrometry.