Discrimination and authentication of lard blending with palm oil in cosmetic soap formulations.

BACKGROUND: The employment of Fourier transforms infrared (FT-IR) spectroscopy combined with chemometrics for determination and quantification of lard in a binary blend with palm oil in a cosmetic soap formulations. OBJECTIVE: To determine and quantify lard as an adulterant in a binary blend with palm oil in a cosmetic soap formulations by FT-IR and multivariate analysis. METHODS: Fatty acids in lard, palm oil and binary blends were extracted via liquid-liquid extraction and were subjected to FTIR spectrometry, combined with principal component analysis (PCA) and discriminant analysis (DA) for the classification of lard in cosmetic soap formulations via two DA models: Model A (percentage of lard in cosmetic soap) and Model B (porcine and non-porcine cosmetic soap). Linear regression (MLR), partial least square regression (PLS-R) and principal components regression (PCR) were used to assess the degree of adulteration of lard in the cosmetic soap. FINDINGS: The FTIR spectrum of palm oil slightly differed from that of lard at the wavenumber range of 1453 cm -1 and 1415 cm -1 in palm oil and lard, respectively, indicating the bending vibrations of CH2 and CH3 aliphatic groups and OH carboxyl group respectively. Both of the DA models could accurately classify 100% of cosmetic soap formulations. Nevertheless, less than 100% of verification value was obtained when it was further used to predict the unknown cosmetic soap sample suspected of containing lard or a different percentage of lard. The PCA for Model A and Model B explained a similar cumulative variability (CV) of 92.86% for the whole dataset. MLR and PCR showed the highest determination coefficient (R2) of 0.996, and the lowest relative standard error (RSE) and mean square error (MSE), indicating that both regression models were effective in quantifying the lard adulterant in cosmetic soap. CONCLUSION: FTIR spectroscopy coupled with chemometrics with DA, PCA and MLR or PCR can be used to analyse the presence of lard and quantify its percentage in cosmetic soap formulations.

CONTEXTE: Combinée à la chimiométrie, la spectroscopie infrarouge à transformée de Fourier (SI-TF) permet de déterminer et de quantifier la présence du saindoux dans un mélange binaire avec de l'huile de palme parmi des formulations de savon cosmétique. OBJECTIF: Déterminer et quantifier le saindoux comme adultérant dans un mélange binaire avec de l'huile de palme parmi des formulations de savon cosmétique par SI-TF et analyse multivariée. MÉTHODES: Les acides gras dans le saindoux, l'huile de palme et les mélanges binaires ont été extraits par extraction liquide-liquide, puis ont été soumis à une SI-TF. Ils ont également fait l'objet d'une analyse en composantes principales (ACP) et d'une analyse discriminante (AD) pour la classification du saindoux dans les formulations de savons cosmétiques via deux modèles d'AD : le modèle A (pourcentage de saindoux dans le savon cosmétique) et le modèle B (savon cosmétique de porc et non de porc). Le degré d'altération du saindoux dans le savon cosmétique a été évalué selon une régression linéaire (régression L), une régression des moindres carrés partiels (régression PLS) et une régression sur composantes principales (régression CP). RÉSULTATS: Le spectre SI-TF de l'huile de palme différait légèrement de celui du saindoux sur la plage de nombre d'ondes de 1 453 cm −1 et 1 415 cm −1 dans l'huile de palme et le saindoux, respectivement, et indiquait les vibrations de flexion des groupes aliphatiques CH2 et CH3, et du groupe carboxyle OH, respectivement. Les deux modèles d'AD ont permis de classer avec précision 100 % des formulations de savon cosmétique. Néanmoins, la valeur de vérification obtenue s'est avérée inférieure à 100 % une fois les modèles utilisés pour prédire l'échantillon de savon cosmétique inconnu suspecté de contenir du saindoux ou un pourcentage de saindoux différent. L'ACP du modèle A et du modèle B expliquait une variabilité cumulée (VC) similaire de 92,86 % pour l'ensemble de l'ensemble des données. La régression L et la régression PLS ont montré le coefficient de détermination le plus élevé (R2), soit 0,996, ainsi que l'erreur type relative (ETR) et l'erreur carrée moyenne (EMM) les plus faibles, indiquant que les deux modèles de régression ont été efficaces pour quantifier le saindoux adultérant dans le savon cosmétique. CONCLUSION: Couplée à la chimiométrie avec une AD, une ACP et une régression L ou une régression PLS, la SI-TF permet d'analyser la présence de saindoux et de quantifier son pourcentage dans les formulations de savon cosmétique.

Volatile compounds, texture, and color characterization of meatballs made from beef, rat, wild boar, and their mixtures.

The purpose of this research was to characterize the volatile compounds, texture, and color profile of meatballs made from beef, rat, wild boar, and their combinations. Volatile compounds were analyzed using SPME/GC-MS and multivariate data analysis (PCA, PLS-DA). Additionally, several textural features such as hardness, gumminess, chewiness, cohesiveness, and colour (L, a∗, b∗, C, and h) were also analyzed. The findings revealed that texture and color characteristics can only be used to differentiate meatballs based on their raw meat materials when meat adulterants are used in high concentrations (≥50%). PLS-DA analysis of volatile data revealed distinct groupings among various types of meatballs, including meatballs adulterated with rat or wild boar meat at the lowest percentage used in this study (20%). By using VIP and correlation coefficient, the strongest markers in beef, rat, and wild boar meatballs were identified as (Z)-2-amino-5-methyl-benzoic acid, 2-heptenal, and cyclobutanol, respectively. Nonanal was consistently found as a significant marker in the meatballs made from a mixture of beef-rat and beef-wild boar at different ratios. This study demonstrated that the volatile profile of meat is more reliable than physicochemical profiles for developing an analytical tool for quickly identifying undesired meat in meat-derived products.

Removal of organochlorine pesticides using zerovalent iron supported on biochar nanocomposite from Nephelium lappaceum (Rambutan) fruit peel waste.

Unique zerovalent iron (Fe0) supported on biochar nanocomposite (Fe0-BRtP) was synthesized from Nephelium lappaceum (Rambutan) fruit peel waste and were applied for the simultaneous removal of 6 selected organochlorine pesticides (OCPs) from aqueous medium. During facile synthesis of Fe0-BRtP, Rambutan peel extract was used as the green reducing mediator to reduce Fe2+ to zerovalent iron (Fe0), instead of toxic sodium borohydride which were used for chemical synthesis. For comparison, chemically synthesized Fe0-BChe nanocomposite was also prepared in this work. Characterization study confirmed the successful synthesis and dispersion of Fe0 nanoparticles on biochar surface. Batch experiments revealed that Fe0-BRtP and Fe0-BChe nanocomposites combine the advantage of adsorption and dechlorination of OCPs in aqueous medium and up to 96-99% and 83-91% removal was obtained within 120 and 150 min, respectively at initial pH 4. Nevertheless, the reactivity of Fe0-BChe nanocomposite decreased 2 folds after being aged in air for one month, whilst Fe0-BRtP almost remained the same. Adsorption isotherm of OCPs were fitted well to Langmuir isotherm and then to Freundlich isotherm. The experimental kinetic data were fitted first to pseudo-second-order adsorption kinetic model and then to pseudo-first-order reduction kinetic model. The adsorption mechanism involves π-π electron-donor-acceptor interaction and adsorption is facilitated by the hydrophobic sorption and pore filling. After being reused five times, the removal efficiency of regenerated Fe0-BChe and Fe0-BRtP was 5-13% and 89-92%, respectively. The application of this Fe0-BRtP nanocomposite could represent a green and low-cost potential material for adsorption and subsequent reduction of OCPs in aquatic system.

A systematic literature review on the current detection tools for authentication analysis of cosmetic ingredients.

BACKGROUND: The use of cosmetic products is considered a necessity for beautification in our daily lives. Cosmetic products composed of natural oils or fats as a main ingredient for various beneficial properties. Fats and oils are composed of various type of fatty acids with different compositions. Hence, fatty acids profile can be an effective chemical fingerprint for authentication analysis of cosmetic products. OBJECTIVE: This systematic review aims to enlighten the current detection tools developing for fatty acids profile authentication analyses of cosmetic ingredients based on the effectiveness, halal status, safety, advantages and disadvantages of the methods. METHODOLOGY: The data were extracted from the scientific literatures published between October 2015 and 2020 in the Web of Science, Scopus and Google Scholar databases, and analyzed with Preferred Reporting Items for Systematic Reviews and Meta-Analyses (PRISMA). FINDINGS: Based on the systemic literature reviews, essential oil, argan oil, mineral oil, vegetable oil, and jojoba oil were among the mostly studied ingredients in cosmetics. Furthermore, a combination of more than one analytical instrument was utilized to profile fatty acids while the determination of the origin of the fatty acids is under scrutiny. The portable mass spectrometer combined with a direct inlet membrane (DIM) probe seems to be the best tool in terms of time consumption, cost, requires no sample preparation with high efficiency. The current review showed that the best cosmetic base is when the oil is composed of high concentration of fatty acids such as linoleic, oleic, stearic acid, and palmitic acids with concentration range from 19.7 - 46.30%, which offers various beneficial properties to cosmetic products.

Molecularly imprinted polymers-based DNA biosensors.

In multiple biological processes, molecular recognition performs an integral role in detecting bio analytes. Molecular imprinted polymers (MIPs) are tailored sensing materials that can biomimic the biologic ligands and can detect specific target molecules selectively and sensitively. The formulation of molecularly imprinted polymers is followed by the formulation of a control termed as non-imprinted polymer (NIP), which, in the absence of a template, is commonly formulated to evaluate whether distinctive imprints have been produced for the template. Given the difficulties confronting bioanalytical researchers, it is inevitable that this strategy would come out as a central route of multidisciplinary studies to create extremely promising stable artificial receptors as a replacement or accelerate biological matrices. The ease of synthesis, low cost, capability to 'tailor' recognition element for analyte molecules, and stability under harsh environments make MIPs promising candidates as a recognition tool for biosensing. Compared to biological systems, molecular imprinting techniques have several advantages, including high recognition ability, long-term durability, low cost, and robustness, allowing molecularly imprinted polymers to be employed in drug delivery, biosensor technology, and nanotechnology. Molecular imprinted polymer-based sensors still have certain shortcomings in determining biomacromolecules (nucleic acid, protein, lipids, and carbohydrates), considering the vast volume of the latest literature on biomicromolecules. These potential materials are still required to address a few weaknesses until gaining their position in recognition of biomacromolecules. This review aims to highlight the current progress in molecularly imprinted polymers (MIPs)-based sensors for the determination of deoxyribonucleic acid (DNA) or nucleobases.

Assessment of denitrification potential for coastal and inland sites using groundwater and soil analysis: the multivariate approach.

In an effort to determine the reason behind excellent nitrate remediation capacity at Kelantan region, a multivariate approach is employed to evaluate extent to which the influence of sea on soil geochemical composition affect variation pattern of groundwater quality. The results obtained from geochemical analysis of paleo-beach soil in coastal site at Bachok revealed multiple redox activity at different soil strata, involving both heterotrophic and autotrophic denitrification. In soil and water analysis, eight of the fourteen hydro-geochemical parameters (conductivity, temperature, soil texture, oxidation reduction potential, pH, total organic carbon, Fe, Cu, Mn, Cl-, SO42-, NO2-, NO3- and PO43-) measured using standard procedures were subjected to multivariate analysis. Evaluation of general variation pattern across the area reveals that the principal component analysis (PCA), hierarchical cluster analysis (HCA) and linear discriminant analysis (LDA) are in consonance with one another on apportioning three parameters (SO42-, Cl- and conductivity) to the coastal sites and two parameters (Fe and NH4+ or NO3-) to inland sites. The step forward analysis of LDA reveals four parameters in order of decreasing significance as Cl-, Fe and SO42-, while the two-way HCA identifies three clusters on location basis, respectively. In addition to the significant data reduction obtained, the results indicate that proximity to sea and location/geological-based influence are more significant than temporal-based influence in denitrification. By extension, the research reveals that influence of labile portion of natural resources is explorable for broader application in other remediation strategies.

Daily exposure to toxic metals through urban road dust from industrial, commercial, heavy traffic, and residential areas in Petaling Jaya, Malaysia: a health risk assessment.

Human health is threatened by significant emissions of heavy metals into the urban environment due to various activities. Various studies describing health risk analyses on soil and dust have been conducted previously. However, there are limited studies that have been carried out regarding the potential health risk assessment of heavy metals in urban road dust of < 63-µm diameter, via incidental ingestion, dermal contact, and inhalation exposure routes by children and adults in developing countries. Therefore, this study evaluated the health risks of heavy metal exposure via ingestion, dermal contact, and inhalation of urban dust particles in Petaling Jaya, Malaysia. Heavy metals such as lead (Pb), chromium (Cr), zinc (Zn), copper (Cu), and manganese (Mn) were measured using dust samples obtained from industrial, high-traffic, commercial, and residential areas by using inductively coupled plasma mass spectrometry (ICP-MS). The principal component and hierarchical cluster analysis showed the dominance of these metal concentrations at sites associated with anthropogenic activities. This was suggestive of industrial, traffic emissions, atmospheric depositions, and wind as the significant contributors towards urban dust contamination in the study sites. Further exploratory analysis underlined Cr, Pb, Cu, and Zn as the most representative metals in the dust samples. In accommodating the uncertainties associated with health risk calculations and simulating the reasonable maximum exposure of these metals, the related health risks were estimated at the 75th and 95th percentiles. Furthermore, assessing the exposure to carcinogenic and non-carcinogenic metals in the dust revealed that ingestion was the primary route of consumption. Children who ingested dust particles in Petaling Jaya could be more vulnerable to carcinogenic and non-carcinogenic risks, but the exposure for both children and adults showed no potential health effects. Therefore, this study serves as an important premise for a review and reformation of the existing environmental quality standards for human health safety.

Highly sensitive and selective determination of malathion in vegetable extracts by an electrochemical sensor based on Cu-metal organic framework.

This article demonstrates the first application of a copper-based porous coordination polymer (BTCA-P-Cu-CP) as a carbon paste electrode (CPE) modifier for the detection of malathion. The electrochemical behavior of BTCA-P-Cu-CP/CPE was explored using cyclic voltammetry (CV) while chrono-amperometry methods were applied for the analytical evaluation of the sensor performance. Under optimized conditions, the developed sensor exhibited high reproducibility, stability, and wide dynamic range (0.6-24 nM) with the limits of detection and sensitivity equal to 0.17 nM and 5.7 µAnMcm-1, respectively, based on inhibition signal measurement. Furthermore, the presence of common coexisting interfering species showed a minor change in signals (<4.4%). The developed sensor has been applied in the determination of malathion in spiked vegetable extracts. It exhibited promising results in term of fast and sensitive determination of malathion in real samples at trace level with recoveries of 91.0 to 104.4%. (RSDs < 5%, n = 3). A comparison of the two studied techniques showed that the HPLC technique is unable to detect malathion when the concentration is lower than 1.8 µM while 0.006 µM is detected with appropriate RSDs 0.2-5.2% (n = 3) by amperometric method. Due to the high sensitivity and selectivity, this new electrochemical sensor will be useful for monitoring trace malathion in real samples.

Development of magnetic porous coordination polymer adsorbent for the removal and preconcentration of Pb(II) from environmental water samples.

A novel porous coordination polymer adsorbent (BTCA-P-Cu-CP) based on a piperazine(P) as a ligand and 1,2,4,5-benzenetetracarboxylic acid (BTCA) as a linker was synthesized and magnetized to form magnetic porous coordination polymer (BTCA-P-Cu-MCP). Fourier transform infrared (FTIR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), field emission scanning electron microscope(FESEM), energy-dispersive X-ray spectroscopy(EDS), CHN, and Brunauer-Emmett-Teller(BET) analysis were used to characterize the synthesized adsorbent. BTCA-P-Cu-MCP was used for removal and preconcentration of Pb(II) ions from environmental water samples prior to flame atomic absorption spectrometry(FAAS) analysis. The maximum adsorption capacity of BTCA-P-Cu-MCP was 582 mg g-1. Adsorption isotherm, kinetic, and thermodynamic parameters were investigated for Pb(II) ions adsorption. Magnetic solid phase extraction (MSPE) method was used for preconcentration of Pb(II) ions and the parameters influencing the preconcentration process have been examined. The linearity range of proposed method was 0.1-100 µg L-1 with a preconcentration factor of 100. The limits of detection and limits of quantification for lead were 0.03 µg L-1 and 0.11 µg L-1, respectively. The intra-day (n = 7) and inter-day (n = 3) relative standard deviations (RSDs) were 1.54 and 3.43% respectively. The recoveries from 94.75 ± 4 to 100.93 ± 1.9% were obtained for rapid extraction of trace levels of Pb(II) ions in different water samples. The results showed that the BTCA-P-Cu-MCP was steady and effective adsorbent for the decontamination and preconcentration of lead ions from the aqueous environment.

Evaluation of heavy metals and environmental risk assessment in the Mangrove Forest of Kuala Selangor estuary, Malaysia.

This study was carried out to evaluate the distribution, enrichment and ecological risk of heavy metals (arsenic (As), zinc (Zn), manganese (Mn), copper (Cu) and lead (Pb)) concentration in Kuala Selangor estuary at the Kuala Selangor Nature Park. The results suggested that As and Pb in sediment were as high as the background value, suggesting the presence of anthropogenic contamination. The risk assessment of sediment Igeo, CD, and PERI, on the other hand, showed low risk of heavy metals in Kuala Selangor estuary. Meanwhile, risk assessment code (RAC) results showed that Mn, As and Zn presented medium to high level of environmental risk. The translocation factor and bioaccumulation factors of heavy metal concentration by mangrove vegetation showed a variety of trends, which indicates the different partitioning and uptake ability of heavy metal in the tissues of different mangrove species. Therefore, underscores the importance of preserving the high diversity of mangroves at securing the health and productivity of the coastal region. These results may play a critical role in facilitating decision makers in managing the sustainability of mangrove forests.

Chemical species of metallic elements in the aquatic environment of an ex-mining catchment.

This study was conducted to investigate the chemical speciation of dissolved and particulate elements (lead, zinc, copper, chromium, arsenic, and tin) in the mining wastewater of a former tin-mining catchment. The speciation patterns of dissolved elements were estimated by an adsorptive stripping voltammeter (ASV), while particulate elements were analyzed by using a newly developed sequential-extraction leaching procedure. The procedure has been operationally defined among five host fractions, namely exchangeable, carbonate, reducible, organic bound, and residual fractions. A total of six elements (lead, zinc, copper, chromium, arsenic, and tin) were analyzed in thirty samples at ten locations (P1-P10), with three samples taken from each of the ten locations, to get the average value from the former tin-mining catchment. The results showed that the heavy metal pollutions in locations P4 and P8 were more severe than in other sampling sites, especially tin and lead pollution. In the water samples from locations P4 and P8, both the total contents and the most dangerous non-residual fractions of tin and lead were extremely high. More than 90% of the total concentrations of arsenic and chromium existed in the residual fraction. Concentrations of copper and zinc mainly occurred in the residual fraction (more than 60%), while lead and tin presented mostly in the non-residual fractions in surface water. For all of the six dissolved elements, the less-labile species formed the predominant fraction in their speciation patterns. The speciation patterns of particulate elements showed that most of the concentrations of zinc, copper, chromium, and arsenic were found in the reducible fraction; whereas lead and tin were mainly associated with the organic fraction.

Determination of polar aromatic amines using newly synthesized sol-gel titanium (IV) butoxide cyanopropyltriethoxysilane as solid phase extraction sorbent.

A solid phase extraction (SPE) method has been developed using a newly synthesized titanium (IV) butoxide-cyanopropyltriethoxysilane (Ti-CNPrTEOS) sorbent for polar selective extraction of aromatic amines in river water sample. The effect of different parameters on the extraction recovery was studied using the SPE method. The applicability of the sorbents for the extraction of polar aromatic amines by the SPE was extensively studied and evaluated as a function of pH, conditioning solvent, sample loading volume, elution solvent and elution solvent volume. The optimum experimental conditions were sample at pH 7, dichloromethane as conditioning solvent, 10 mL sample loading volume and 5 mL of acetonitrile as the eluting solvent. Under the optimum conditions, the limit of detection (LOD) and limit of quantification (LOQ) for solid phase extraction using Ti-CNPrTEOS SPE sorbent (0.01-0.2; 0.03-0.61 µg L(-1)) were lower compared with those achieved using Si-CN SPE sorbent (0.25-1.50; 1.96-3.59 µg L(-1)) and C18 SPE sorbent (0.37-0.98; 1.87-2.87 µg L(-1)) with higher selectivity towards the extraction of polar aromatic amines. The optimized procedure was successfully applied for the solid phase extraction method of selected aromatic amines in river water, waste water and tap water samples prior to the gas chromatography-flame ionization detector separation.

A simple and efficient multi-residue method based on QuEChERS for pesticides determination in palm oil by liquid chromatography time-of-flight mass spectrometry.

In this study, a rapid, specific and sensitive multi-residue method based on acetonitrile extraction followed by dispersive solid-phase extraction (d-SPE) clean-up was implemented and validated for multi-class pesticide residues determination in palm oil for the first time. Liquid-liquid extraction followed by low-temperature precipitation procedure was evaluated in order to study the freezing-out clean-up efficiency to obtain high recovery yield and low co-extract fat residue in the final extract. For clean-up step, d-SPE was carried out using a combination of anhydrous magnesium sulphate (MgSO(4)), primary secondary amine, octadecyl (C(18)) and graphitized carbon black. Recovery study was performed at two concentration levels (10 and 100 ng g(-1)), yielding recovery rates between 74.52% and 97.1% with relative standard deviation values below 10% (n = 6) except diuron. Detection and quantification limits were lower than 5 and 9 ng g(-1), respectively. In addition, soft matrix effects (≤±20%) were observed for most of the studied pesticides except malathion that indicated medium (20-50%) matrix effects. The proposed method was successfully applied to the analysis of suspected palm oil samples.

Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 µg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia.

Speciation of heavy metals by modified BCR sequential extraction procedure in different depths of sediments from Sungai Buloh, Selangor, Malaysia.

The sequential extraction procedure proposed by the European Standard, Measurements and Testing (SM&T) program, formerly the Community Bureau of Reference (BCR), was applied for partitioning of heavy metals (HMs) in river sediments collected along the course of Sungai Buloh and the Straits of Malacca in Selangor, Malaysia. Eight elements (V, Pb, Cd, Cr, Co, Ni, Cu and Zn) from seven stations (S1-S7) and at different depths were analyzed using the modified BCR Sequential Extraction Procedure (SEP) in combination with ICP-MS to obtain the metal distribution patterns in this region. The results showed that heavy metal contaminations at S2 and S3 was more severe than at other sampling sites, especially for Zn, Cu, Ni and Pb. Nevertheless, the element concentrations from top to bottom layers decreased predominantly. The samples from the Straits of Malacca (S4-S7) the highest contamination factors obtained were for Co, Zn and Pb while the lowest were found for V and Cr, similar to Sungai Buloh sediments. The sediments showed a low risk for V, Cr, Cu and Pb with RAC values of less than 10%, but medium risk for Co, Zn (except S3), Cd at S1 and S2 and Ni at S1, S3 and S5. Zn at S3 and Cd at S3-S7 showed high risk to our sediment samples. There is not any element of very high risk conditions in the selected samples.

Low temperature followed by matrix solid-phase dispersion-sonication procedure for the determination of multiclass pesticides in palm oil using LC-TOF-MS.

A simple and effective multiresidue method based on precipitation at low temperature followed by matrix solid-phase dispersion-sonication was developed and validated to determine dimethoate, malathion, carbaryl, simazine, terbuthylazine, atrazine and diuron in palm oil using liquid chromatography time-of-flight mass spectrometry (LC-TOF-MS). Liquid-liquid extraction (LLE) followed by low temperature method were optimized by studying the effect of type and volume of organic solvent (acetonitrile, acetonitrile:n-hexane (3:2 v/v) and acetone) and time of freezing to obtain high recovery yield and low co-extract fat residue in the final extract. The optimal conditions for matrix solid-phase dispersion (MSPD) were obtained using 5 g of palm oil, 2 g of primary secondary amine (PSA) as dispersing sorbent, 1 g of graphitized carbon black (GCB) as clean-up sorbent and 15 mL of acetonitrile as eluting solvent under conditions of 15 min ultrasonication at room temperature. Method validation was performed in order to study sensitivity, linearity, precision, and accuracy. Average recoveries at three concentration levels (25, 50 and 100 µg kg(-1)) were found in the range of 72.6-91.3% with relative standard deviations between 5.3% and 14.2%. Detection and quantification limits ranged from 1.5 to 5 µg kg(-1) and from 2.5 to 9 µg kg(-1), respectively.

Comparison of unmodified and modified BCR sequential extraction schemes for the fractionation of heavy metals in shrimp aquaculture sludge from Selangor, Malaysia.

A study was carried out to investigate the fractionation of Cd, Cr, Cu, Fe, Mn, Pb, and Zn in shrimp aquaculture sludge from Selangor, Malaysia, using original (unmodified) and modified four-steps BCR (European Community Bureau of Reference, now known as the Standards Measurements and Testing Program) sequential extraction scheme. Step 2 of the unmodified BCR procedure (subsequently called Method A) involves treatment with 0.1 M hydroxylammonium chloride at pH 2, whereas 0.5 M hydroxylammonium chloride at pH 1.5 was used in the modified BCR procedure (subsequently called Method B). Metal analyses were carried out by flame atomic absorption spectrometry. A pseudo-total aqua-regia digest of BCR CRM 701 has also been undertaken for quality assurance purposes. The recovery of Method A for all metals studied ranges from 96.14% to 105.26%, while the recovery for Method B ranges from 95.94% to 122.40%. Our results reveal that Method A underestimated the proportion of metals bound to the easily reducible fraction except for copper. Therefore, the potential mobility of these elements is higher than others. Thus, to use this sludge as a fertilizer we have to first find a remediation for reduction of heavy metal contamination.

Comparative study on open system digestion and microwave assisted digestion methods for metal determination in shrimp sludge compost.

The aim of this work was to evaluate two different digestion methods for the determination of the total concentration of metals (Zn, Cu, Cr, Ni, Pb and Cd) in shrimp sludge compost. The compost made from shrimp aquaculture sludge co-composted with organic materials (peat, crushed bark and manure) was used as an organic growing medium for crop. Open system digestion and microwave assisted digestion procedures were employed in sample preparation. Various combinations and volumes of hydrofluoric, nitric and hydrochloric acids were evaluated for the efficiency of both methods. A certified reference material (CRM 146) was used in the comparison of these two digestion methods. The results revealed a good agreement between both procedures and the certified valued. The best recoveries were found in the range between 95% and 99% for microwave assisted digestion with a mixture of 2 ml of HF, 6 ml of HNO(3) and 2 ml of HCl. This procedure was recommended as the method for digestion the compost herein based on the recovery analysis and time taken.

Multi-residue analysis of pharmaceutical compounds in wastewaters by dual solid-phase microextraction coupled to liquid chromatography electrospray ionization ion trap mass spectrometry.

The aim of this article is to present a new procedure based on dual solid-phase microextraction (dSPME) for the simultaneous extraction of 16 pharmaceutical compounds with acidic and basic characteristics in urban wastewaters. Water samples are divided into two aliquots of 2 mL each extracted by two CW-TPR fibers at different pH values (pH 3 and 11) and with a NaCl concentration of 300 g L(-1) at 75 degrees C for 30 min. The analytes in both fibers are desorbed one after the other in the desorption chamber in static mode with mobile phase for 10 min. The extracts are injected into an LC system coupled to an ion trap mass spectrometer, leading to the accurate quantification of 16 pharmaceutical compounds in wastewaters, in MS(2) mode. All the target compounds found in wastewaters provide good signals corresponding to the protonated precursor ion [M+H](+). The parameters influencing adsorption and desorption of the analytes on fiber were optimized. The assessment of the analytical method was performed by studying the linearity (LOQ to 10 ng mL(-1)) and the intra- and interday accuracy (89.2-109.7%) and precision (RSD <13.6%). The quantification limits obtained ranged between 0.005 and 0.05 microg L(-1). The application of the method to real samples proves its effectiveness in identifying and detecting naproxen, valsartan, bezafibrate, torasemide, diclofenac, carbamazepine, citalopram, lorazepan, fluoxetine, imipramine and amitriptyline in influent and effluent wastewater treatment plant samples.