Florisil Column Research Articles

Polycyclic aromatic hydrocarbons in sewage-irrigated vegetables from industrial cities in Haryana, India.

The majority of Indians consume a lot of vegetables because of their health advantages. High concentrations of polycyclic aromatic hydrocarbons (PAHs) in vegetables may be seriously harmful to consumers' health. The method for identifying and measuring 16 USEPA polycyclic aromatic hydrocarbons (PAHs) in samples of sewage-irrigated vegetables from three industrial cities in Haryana, India, is described in this research. Ultrasonication, liquid-liquid extraction using n-hexane as a solvent, clean-up using a Florisil column, and reversed-phase high-performance liquid chromatography with a UV detector were all included in the process. The PAHs were successfully linearized (R2 > 0.99) at various doses. Results for PAH recovery ranged from 90 to about 100%. The limit of quantification was 0.002-0.580, and the limit of detection was 0.0006-0.174 µgkg-1. Data indicated that the highest mean concentrations of ∑16 PAHs were detected in Spinach (123.36 µgkg-1), in carrot (105.09 µgkg-1), and in cucumber (63.40 µgkg-1) among leafy, underground, and fruity vegetables, respectively.

Distribution, Associated Risks and Sources of Organochlorine Pesticides in Farmland Soils from Ethiope West Area of Delta State, Nigeria

rganochlorine pesticides (OCPs) usage provides many advantages for agriculture; however, there are also significant concerns to the environment and public health. Since there is little information available on OCPs' distribution, associated risks and sources in Nigerian farmland soils, this study was carried out. Soil samples were collected from farmlands in ten communities. Samples were extracted with hexane/dichloromethane and cleaned up in a column of silica gel and florisil. The OCPs were measured using a gas chromatograph-mass spectrometry (GC-MS). The ∑20 OCPs levels in the soils varied between 47.5 and 109 ng/g. The OCPs homologues distribution in the soils was in the order of ∑DDTs > ∑Drins > ∑Chlordane > ∑BHCs > ∑Endosulfan. The risks assessment result indicated that there was adverse ecological effect on organisms residing in the soils and there is the likelihood that this effect will be frequently observed. Moreover, there was potential non-carcinogenic and carcinogenic risks for persons exposed to OCPs in these farmland soils. The result of the source identification indicated that historical usage was the main source of OCPs in these farmland soils. Keywords: Soil, Farmland, OCPs, Non-carcinogenic, Carcinogenic, Ethiope West

Maternal serum dioxin-like activity and gestational age at birth and indices of foetal growth: The Aarhus birth cohort

Human exposure to lipophilic persistent organic pollutants (lipPOP) is ubiquitous and life-long, beginning during foetal development. Exposure to lipPOP elicits a number of species and tissue specific responses including dioxin-like activity which involve the activation of aryl hydrocarbon receptor (AhR). This study aims i) to describe the combined dioxin-like activity in serum from Danish pregnant women collected during 2011–2013; ii) to assess the association between maternal serum dioxin-like activity, gestational age at birth and foetal growth indices.The serum lipPOP fraction was extracted using Solid Phase Extraction and cleaned-up on Supelco multi-layer silica and florisil columns. The combined dioxin-like activity of the extract was determined using the AhR reporter gene bioassay, expressed as 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) toxic equivalent (TEQ) [AhR-TEQ (pg/g lipid)]. The associations of AhR-TEQ and foetal growth indices (birth weight, birth length and head circumference) and gestational age were assessed by linear regression models.We detected AhR-TEQ in 93.9 % of maternal first trimester serum samples, with a median level of 185 pg/g lipid. Each ln-unit increase in AhR-TEQ was associated with an increase in birth weight of 36 g (95 % CI: 5; 68), birth length of 0.2 cm (95 % CI: 0.01; 0.3) and pregnancy duration of 1 day (95 % CI: 0; 1.5). In women who never smoked, higher AhR-TEQ values were associated with higher birth weight and longer duration of gestation, while in smokers the association was the opposite. Mediation analyses suggested that gestational age may mediate the association of AhR-TEQ with foetal growth indices.We conclude that AhR activating substances are present in the bloodstream of almost all pregnant women in Denmark and the AhR-TEQ level was around four times higher than previously reported. The AhR-TEQ was associated with slightly longer gestational duration and thereby higher birth weight and birth length.

A new simpler and reliable method for determining mineral oil in sewage sludge: Influence of biogenic compounds for the quantitative analysis of C10–C40 hydrocarbons

The characterization of organic contaminants in sewage sludge is a fundamental step to address the relevant most appropriate management practice. In this perspective, C10–C40 hydrocarbon content was considered in Italy a crucial parameter to be considered, in spite of its irrelevance in the literature. The very complex mixture of organic substances of both biogenic and anthropogenic origin the sludge is made up of makes sewage sludge a matrix of uniqueness nature, and the analytic determination of hydrocarbon content through conventional procedures may be subjected to overestimation. In this work, optimization of two conventional protocols for the determination of mineral oil (EN14039 and IRSA CNR gravimetric method) were run with attention to anthropogenic compounds potentially affecting the C10–C40 mineral hydrocarbons determination. Effects from the first manipulations of sewage sludge samples to extraction procedure and clean-up operations were investigated.A new simple procedure was set up and tested on 30 samples from different wastewater treatment plants (WWTPs). Through a simple extraction with hexane (12 mL per 2 g of dried sludge, acidified with HCl conc.) at room temperature for 2 h, followed by a clean-up on Florisil column (10 mL–2 g) a confident determination of C10–C40 were obtained with respect to conventional optimized procedures. Variability within the range 0.06–9.49% was calculated with respect to the average value determined using three different methods, with an average value of 2.48 ± 2.37%, demonstrating the robustness of the determination. Up to 3% of the total hydrocarbons were identified as naturally occurring, namely terpenes, squalenes and deoxygenized sterols, passed through the clean-up Florisil column. A significant incidence (up to 75%) of the final overall C10–C40 content was found to be related to the C10–C20 component, originally present in the commercial polyelectrolytes in emulsion, widely used for conditioning before mechanical dewatering.

Screening of risky substances in sea cucumbers based on gas chromatography-orbitrap high-resolution mass spectrometry

建立了一种基于改良QuEChERs的样品前处理新方法,并通过气相色谱-静电场轨道阱高分辨质谱(GC-Orbitrap HRMS)对海参样品中的有机氯农药类(OCPs)、多环芳烃类(PAHs)、酞酸酯类(PAEs)、多氯联苯类(PCBs)及其他农药类(ACs)等10大类289种具有健康风险的有机污染物进行了高通量高精准的定性鉴别和定量分析。通过将传统的QuEChERs方法与柱净化方法结合,提出了一种基于改良QuEChERs的简便生物样品制备新方法,经弗洛里硅土(Florisil)柱净化后脂含量降低了99.9%,显著减少了基质效应对分析结果的干扰,可在高分辨质谱(6万分辨率)全扫描模式下对289种目标化合物同时进行高精准定性筛查和定量分析。该方法定量限约0.56~57.8 pg/g,线性范围约6个数量级,回收率范围为40%~120%。由于Q Exactive GC-Orbitrap HRMS具备较高的质量分辨率和灵敏度,因此对目标化合物的定量限显著优于常规的色谱和质谱分析方法,常规方法无法检出的超痕量有机污染物利用该研究开发的方法可进行精准定量。基于此高覆盖度多目标分析方法对养殖场采集的海参样品进行分析,共从海参体内检出100种有机污染物,其中PAHs、ACs、PAEs、OCPs类检出总含量相对高于其他类污染物,总含量均值分别为157.8、153.2、64.4和46.4 ng/g dw。9-氯芴、5-氯苊、3-甲基胆蒽等多种新污染物首次在海参样品中检出,但含量都非常低。该方法简单高效,定量限低,线性范围宽,结果准确。此高覆盖度多目标分析方法可广泛应用于各种水产品中风险物质的广谱筛查和精准定量,为食品安全和绿色养殖提供技术支撑。

Effect of gamma rays and accelerated electron beam on medullary lipids decomposition: influence of dose and irradiation temperature.

Ionizing radiation sterilization of non-defatted bone grafts has been found to deteriorate their quality and biocompatibility due to induction of lipid peroxidation products toxic for osteoblast-like cells. Therefore, the purpose of our study was to evaluate the effect of two types of ionizing radiation-gamma rays (G) or accelerated electron beam (EB) applied with two doses at different temperature conditions on hydrocarbons production, resulting from decomposition of palmitic and oleic acids-most abundant fatty acids in medullary lipids. Bone marrow samples isolated from femoral shafts of 6 male donors (aged 46-67 years) were irradiated with G or EB with doses of 25 or 35kGy at different temperature conditions (ambient or deep freezing temperature). Fresh-frozen, non-irradiated samples served as control. Marrow lipids were extracted with n-hexane (Soxhlet's method), hydrocarbons fraction isolated on Florisil column chromatography, separated by gas chromatography and detected by mass spectrometry. Irradiation of bone marrow with sterilization doses of ionizing radiation (G and EB) was found to induce lipid radiolysis as measured by resulting hydrocarbons production. The effect was dose-dependent, whereas no marked influence of radiation type was observed. In contrast, irradiation temperature had a profound effect on lipids decomposition which was partially prevented while irradiation was performed in deep frozen state. Defatting of bone grafts prior to ionizing radiation sterilization seems essential for their biocompatibility, whereas irradiation in a deep-frozen state might compromise the effectiveness of sterilization and needs further studies.

Analytical research on the separation and residue of chiral pesticide triadimenol in fruit and vegetable puree.

In this paper, a method for the separation of triadimenol stereoisomers using ultra-performance convergence chromatography and an analytical method for the determination of triadimenol stereoisomer residues in pumpkin puree, apple puree, and tomato puree as a supplement for infants are established. Test samples were extracted with acetonitrile and successively purified with graphitized carbon black and Florisil column. Afterward, Acquity Trefoil AMY1 column was adopted for chiral separation of chromatographic column, and gradientelute was carried out with supercritical carbon dioxide-methanol as the mobile phase and with external standard method for quantitation. Results showed that the linearly dependent coefficient of the four kinds of triadimenol stereoisomers within 1.0 and 50mg/L was greater than 0.9997, and the limit of quantitation of the four kinds of triadimenol stereoisomers was 0.05mg/kg. Recovery experiment was carried out within 0.05 and 1.0mg/kg scope, the recoveries were 81.0-107％, and the relative standard deviation was 2.3-7.6%. This method implemented the separation of triadimenol stereoisomers and its residue test in pumpkin puree, apple puree, and tomato puree as a supplement for infants, and it can provide reliable technical support for the analysis of pesticide residue and assessment of product quality.

Development of SPE clean-up procedure for acrylamide determination from potato-based products by GC-MS/MS

Abstract The aim of this work was to develop an analytical method for determining acrylamide in potato-based products by gas chromatography and tandem mass spectrometry analysis (GC-MS/MS) using solid-phase extraction (SPE) clean-up. Different conditions for extraction and clean-up of AA extracts were studied on a potato crisps reference material (RM) with the value of 625 ± 45 μg/kg: the solvent volume used for AA elution, the extraction water temperature, the volume of hexane used, and also the addition of Carrez solutions. The SPE cartridge sorbents contain silica-based C-18 groups (anion and cation exchangers) and polymers (polystyrene-divinylbenzene). After SPE clean-up, extracts were derivatized with bromine compounds. A good efficiency for AA extraction and a cleaned-up extract from this matrix were obtained when the SPE procedure was carried out with water at room temperature, simultaneous with hexane, without Carrez solutions, by using two types of SPE cartridges (Isolute Multimode; Isolute ENV+), and 5 mL of elution solvent. The SPE clean-up procedure functionality was demonstrated by the results obtained in the Food Analysis Performance Assessment Scheme proficiency test (z-score: −0.8) on French fries (precooked) matrix and also by comparative analysis with a laboratory procedure, validated and accredited on cereal-based food matrices, in which liquid–liquid extraction and clean-up through a florisil column were realized (RSD(R) = 2.23–5.10%).

Determination of aldicarb, propoxur, carbofuran, carbaryl and methiocarb residues in honey by HPLC with post-column derivatization and fluorescence detection after elution from a florisil column

Determination of aldicarb, propoxur, carbofuran, carbaryl and methiocarb residues in honey by HPLC with post-column derivatization and fluorescence detection after elution from a florisil column

Studies on the Analysis of Ethopabate in Chicken Meat and Livers

A high performance liquid chromatographic(HPLC) method for the determination of ethopabate in chicken meat and river was developed. Ethopabate was extracted from samples with acetonitrile, and filtered. The extract was partitioned with n-hexane, concentrated to dryness, cleaned up through Florisil column, and quantitatively analyzed by HPLC. A Lichrospher 100 PR-18 (25cm x 4. 6 mm i.d., packed with 5 um particle size) and a solvent system of acetonitrile/water (3/7)with a flow rate of 1.0 mi/min were used. Ethopabates were detected by fluorescence with excitation and emission wavelengths at 300 nm and 350 nm, respectively. The average recoveries of ethopabate spiked into samples at the levels of 0. 02,0.05, 0.10 and 0. 20 ppm were in range of 93.22-94. 67% from meat and 92.77 - 94.45% from liver. Coefficients of variation were less than 4%. The detection limit was 2 ppb. Twenty-five samples each of chicken meat and liver purchased from various markets in Taipei were investigated. Results showed that no ethopabate was detected.

Determination of organochlorine and nitrogen-containing pesticide residues fish with different fat content

A rapid and multiresidue method for determination the residues of organochlorine and nitrogen-containing pesticides in the different fat content fish by solid-phase extraction (SPE) technique was developed. In the present procedures, samples were extracted with acetonitrile. The extracts were cleaned up by a tandem SPE column of C18 and florisil, using acetonitrile as the only solvent. Residues were determined by gas chromatography equipped with electron capture detector. Recovery was obtained by three concentration levels of 12 organochlorine pesticides and their metabolites (chlorobenzilate, dieldrin, endosulfan sulfate, endosulfan, endrin, heptachlor, heptachlor epoxide, lindane, methoxchlor, p,p'-DDE, p,p'-DDT) and two nitrogen-containing pesticides (alachlor and trifluralin) from 9 fishes with 1.2-23.3% of fat content, respectively. The recoveries of the spiked pesticides residues from the fishes of different fat contain (fat < 10%, fat ≥ 10 but < 20%, and fat ≥ 20%) were in the range from 73.4% to 119.6%. There were no significant difference in the recovery between pesticides concentration and fat content. The recoveries of two samples were not included because of coutaminated by p,p'-DDT and endosulfan separately, or disruption by sample matrix.

Determination of 14 Lipophilic Pesticide Residues in Raw Propolis by Selective Sample Preparation and Gas Chromatography–Tandem Mass Spectrometry

A selective and reliable method was developed and validated for the determination of 14 lipophilic pesticides in raw propolis by gas chromatography–tandem mass spectrometry (GC-MS/MS) analysis. A test portion of milled sample was extracted with n-hexane followed by back extraction with acetonitrile and cleanup using EMR-Lipid and Florisil column adsorption. Matrix-matched standards were used to compensate for matrix effects. Typical linear correlation coefficients (R2) were ≥ 0.989 in concentration range of 0.001–0.200 μg/mL. Method validation was carried out at three spiking levels and three individual days, and it was found that the mean interday average recoveries were 61.0–106.8% with relative standard deviations ≤ 16.9%. Limits of quantification were ranged from 0.002 to 0.020 μg/g. Analysis of market propolis samples showed contamination by pesticides (e.g., tau-fluvalinate) to some degree.

Nivoi nekih organskih zagađivača u uzorcima vode Jadranskog mora - studija slučaja - žarište Porto-Romana, Albanija

This paper presents concentrations of organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs) and polycyclic aromatic hydrocarbons (PAHs) in marine water samples of Porto-Romano area. Porto-Romano is situated in Adriatic Sea, near city of Durres, in central Albania. It was considered Hot-spot area because before 90' there was located chemical plant for Lindane production. Landfill near Porto-Romano and elevated activity for industrial development of this area can be the main sources of water pollution in recent years. Water samples were taken in December 2018 and April 2019 in nine stations of Porto-Romano. Liquid-liquid extraction was used for isolate organic pollutants from water samples. Clean-up procedure for chlorinated pollutants was realized in a Florisil column. Qualitative and quantitative analyzes of pesticides and PCBs were performed in HP 6890 Series II, gas chromatograph equipped with p-ECD detector. For separation of organochlorine pollutants was used Rtx-5 capillary column. Analyzes of PAH were realized in Varian 450 GC, gas chromatograph equipped with FID detector and VF-1ms capillary column. The most frequent organic pollutants in water samples of Porto-Romano were found organochlorine pesticides because of ex-chemical plants impact in this area. Note, that Lindane and its isomers weren't found in high concentration. PCB 28, volatile congener, was found in higher concentrations because of their atmospheric origin. Presence of PCB 138 show terrestrial origin of PCBs in this area. PAH were found in higher concentrations inside of hydrocarbon port. Their concentrations were due to industrial activity and ship transport in this area. Mismanagement of Lindane plant wastes, urban pollution and recent industrial activity are factors of continues pollution in Porto-Romano area. Presence of organic pollutants in water samples of Porto-Romano indicates that monitoring of this Hot-spot should be continuous.

Photolytic Transformation Products of Decabromodiphenyl Ethane (DBDPE).

The photolytic transformation of decabromodiphenyl ethane-a current-use brominated flame retardant and major substitute of the structurally related decabromodiphenyl ether-was investigated in different solvents (toluene, dichloromethane, chlorobenzene, and benzyl alcohol). The transformation rate followed pseudo first order kinetics, with increasing half-life ( t1/2) in the order of toluene ( t1/2 = 4.6 min), chlorobenzene ( t1/2 = 14.0 min), dichloromethane ( t1/2 = 27.9 min), and benzyl alcohol ( t1/2 ≈ 60 min). Formation and amount of transformation products varied depending on the solvent used. A detailed study of the hydrodebromination products allowed us to tentatively assign all three possible nonaBDPEs (BDPE 207, 208, and in benzyl alcohol only BDPE 206) and three predominant octaBDPE congeners (BDPE 197, 201, and 202). Next to the reported BDPEs, formation of several oxygen containing transformation products (OxyTPs), dominated by octabrominated OxyTP, was verified by GC-Orbitrap-HRMS analysis. Use of HPLC and Florisil column enabled the separation of OxyTPs and BDPEs, and the polybrominated OxyTPs were most likely tricyclic compounds with almost planar structure.

Determination of pyrethroid pesticides in tea by accelerated solvent extraction and ultra-performance liquid chromatography-tandem mass spectrometry

A method was developed for the determination of pyrethroid pesticides in tea by accelerated solvent extraction (ASE) combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted from tea using n-hexane and acetone (2:1, v/v) for 5 min at 10.34 MPa and 80℃ via a single cycle of accelerated solvent extraction. The extract was purified by GCB/NH2 and Florisil columns, analyzed by UPLC-MS/MS in positive electrospray ionization (ESI+) and multiple reaction monitoring (MRM) modes, and quantified by the external standard method. Regression analysis revealed that the linear relationships between mass concentration and peak area are significant for the 10 pyrethroid pesticides, and the correlation coefficients (r) are all not less than 0.9995. The limits of detection (LOD) of the 10 pyrethroid pesticides ranged from 0.5 μg/kg to 5.0 μg/kg and the limits of quantification (LOQ) ranged from 1.6 μg/kg to 16.6 μg/kg. The recoveries of all the pesticides ranged from 68.7% to 103.8% at the spiked levels of LOQ, 0.4 mg/kg and maximum residue limit (MRL) (added 1 mg/kg without MRL) with RSDs ranging from 0.8% to 13.2% (n=7). The proposed method is simple, rapid, sensitive, and accurate, and could be effective for trace analysis of pyrethroid pesticides in tea.

Analysis for Organochlorine Pesticide Residues in Honey from Kabale District, South-Western Uganda

This study was motivated by the reported accumulation of Organochlorine Pesticides (OCPs) residues in the various environmental matrices within Uganda, resulting from their use in agriculture and health sectors. This raised a concern of the likelihood of the accumulation of the OCPs residues in the honey produced within the country which would affect its purity as well as quality and consequently its competition on the world market. Sixty representative honey samples were collected from selected local beekeepers from four sampling stations in Muko sub-county, Kabale, and extracted for OCPs using a solid-phase procedure followed by a florisil column packed clean-up method and Gas Chromatography-Electron Capture Detector (GC-ECD) analysis. Confirmation of the selected samples was done using an Agilent (6890N, USA) gas chromatograph combined with a mass spectrometer. Recoveries of spiked samples ranged from 71% to 96%, except for pp-DDE (54%), with relative standard deviations from 2% to 14% in terms of repeatability, and from 4% to 17% in terms of reproducibility. Limits of quantification were from 0.003 to 0.1 mg·kg-1. Endosulfan sulfate was the most frequently detected in 38% of the samples, followed by HexaChloroBenzene (Lindane) in 21% of the samples. Residues of DDT and their metabolites were detected in 17% of the samples. Mean concentrations of the pesticide residues detected range from ND (not detected) to 1.53 μg/Kg. The acceptable Maximum residual limits (MLRs) are 200 - 300 μg·kg-1 fresh weight for dieldrin, 500 μg·kg-1 for DDT and break down products, and 50 μg·kg-1 wet weight for Lindane (WHO/FAO 2011). Results indicate that the levels of OCP residues detected in honey from the country’s South Western District of Kabale were within the acceptable limits, and hence this honey was safe for human consumption.

A new multistep purification method for simultaneously determining organic ultraviolet absorbents in fish tissue.

More information is required to improve our understanding of the presence of organic ultraviolet absorbents (UVAs) in organisms and the risks posed to biota. Effective removal of lipids in the determination of UVAs in biological samples is a sample-processing bottleneck. In this study, we optimized a multistep purification method for fish tissue samples extracted using an ultrasonic-assisted extraction method. The purification method involved performing Florisil column chromatography, redissolving the extract in ethanol, and then performing dispersive solid-phase extraction using primary and secondary amine, Florisil, and C18 silica sorbents. The purified samples were analyzed by gas chromatography-mass spectrometry. The method was effective and reliable, and was used to detect trace concentrations (ng/g) of 12 UVAs in fish tissue samples. The mean recovery range of the UVAs in fish tissue extracts was 65.4-118%, and the method detection limit range was 0.20-2.50ng/g dw. The validated method was used to analyze 12 UVAs in fish samples from a local supermarket.

A clean-up method for determination of multi-classes of persistent organic pollutants in sediment and biota samples with an aliquot sample

In the present study, we developed a novel method to simultaneously detect eight classes of persistent organic pollutants (POPs), including polychlorinated biphenyls (PCBs), polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs), polybrominated dibenzo-p-dioxins and dibenzofurans (PBDD/Fs), polychlorinated naphthalenes (PCNs), organochlorine pesticides (OCPs), short-chain chlorinated paraffins (SCCPs) and Dechlorane Plus (DP), in sediment and fish tissue samples. The samples were extracted by accelerated solvent extraction (ASE) system, and the extracts were purified and fractionated into fraction1 and fraction2 with multi-layer silica gel column, followed by further fractionation using a basic alumina column (fraction1) and a Florisil column (fraction2), respectively. Finally, fractions were analyzed with different chromatographic columns and different detectors according to the properties of a chemical compound. The limit of detection for eight classes of POPs ranged from 1 to 30 pg/gdw in fish tissue samples, and from 1 to 33 pg/gdw in sediment samples, except for SCCPs (from 5.6 to 7.6 ng/g in fish tissue samples, and from 1.2 to 8.3 ng/gdw in sediment samples). The recoveries of eight classes of POPs spiked in fish tissue and sediment samples ranged from 43% to 120%, and from 45% to 115%, respectively. The relative standard deviation (RSD) was less than 25%. The accuracy of method was satisfactorily demonstrated by analysis of standard reference materials NIST SRM 1649b and WMF-01. In addition, the newly developed method was successfully applied for analysis of sediment and fish samples collected from the Baiyangdian Lake.

Determination of polybrominated diphenyl ethers in human serum by gas chromatography – inductively coupled plasma mass spectrometry

Polybrominated diphenyl ethers (PBDEs) are flame retardants that are added to a wide range of consumer products. Due to their extensive use in the past, their presence has been documented in multiple environmental compartments and living organisms, including humans. To assess the exposure of humans to PBDEs, a new simple, reliable, and sensitive method was developed for the determination of six PBDE congeners (BDE 28, BDE 47, BDE 99, BDE 100, BDE 153, BDE 154) in human serum by gas chromatography–inductively coupled plasma mass spectrometry (GC-ICP-MS). The PBDEs were extracted from 1 mL ofserum by 30 min of mechanical shaking with formic acid. Subsequently, 2 mL of iso-octane was added and 30 min of mechanical shaking was applied. For clean-up of the extract Florisil column was applied. The analytical method was validated by analysis of human serum standard reference materials SRM 1957 (Non-Fortified Human Serum) and SRM 1958 (Fortified Human Serum). Good agreement of the determined concentrations with those certified was found. The repeatability and reproducibility of the analytical method was within 5.9% and 6.1%, respectively, whereas the limits of detection (LODs) for the PBDEs analysed were between 0.0016 and 0.0039 ng mL−1 wet weight (ww). The feasibility of the method was tested by analysing human serum samples. In this study, the determined concentrations in sera were in a range similar to that of as those reported for certain other European countries.

Determination of 11 synthetic musks in imported seafood by solid phase extraction and gas chromatography-mass spectrometry

A method has been developed for the simultaneous determination of 11 synthetic musks (cashmeran, celestolide, phantolide, musk ambrette, traseolide, galaxolide, musk xylene, tonalide, musk moskene, musk tibetene, and musk ketone) in imported seafood. The method combines solid phase extraction and gas chromatography-mass spectrometry. Samples were extracted by n-hexane and purified using a Florisil column. Internal standards were used to correct for matrix effects. The calibration curves showed good linearity with correlation coefficients greater than 0.99. The limits of detection (S/N>3) ranged from 0.35 to 2.08 μg/kg, and the limits of quantification (S/N>10) were between 1.18 and 5.00 μg/kg. The average recoveries measured at three spiked levels (10, 20, and 30 μg/kg) were in the range 83.1%-117%, with relative standard deviations ranging from 5.1% to 8.5%. Further, the concentrations of 11 synthetic musks in 30 imported seafood in Shanghai were investigated. Galaxolide was detected in 93.3% of samples analysed, in concentration as high as 3.82 μg/kg. Musk ambrette and musk moskene were found in concentrations as high as 15.4 μg/kg and 10.5 μg/kg, respectively. The established method demonstrates high sensitivity and selectivity for the determination and confirmation of 11 synthetic musks in imported seafood.