Development of a syringe membrane-based microextraction method based on metal-organic framework mixed-matrix membranes for preconcentration/extraction of polycyclic aromatic hydrocarbons in tea infusion.

Inevitably, the residues of polycyclic aromatic hydrocarbons (PAHs) in tea leaves will be transferred to hot tea infusion, constituting a certain drinking risk; consequently, it is imperative to develop rapid, sensitive, and robust approaches for their trace-level detection. Herein, we developed a syringe membrane-based microextraction (SMME) method for preconcentration/extraction of PAHs in tea infusions. This method utilized metal-organic framework-mixed matrix membranes (MOF-MMMs) as adsorbents, which anchored the nanoparticles of MOFs onto the surface of PVDF membrane. The UiO-66 (Zr)-based MMM possessed high Brunauer-Emmett-Teller (BET) surface area (320.5 m2 g-1) and pore volume (0.18 cm3 g-1), thus enhancing extraction/adsorption efficiency. Under optimized conditions, the limits of detection for PAHs reached as low as 0.02-0.08 µg L-1 with extraction recoveries of 85.5-102.1%, and the inter-day and intra-day precision was lower than 8.4% in tea infusions. Consequently, the SMME/HPLC-DAD method shows a great potential in conventional monitoring of PAHs in tea samples.

Features of sample preparation techniques in the total-reflection X-ray fluorescence analysis of tea leaves.

Tea is a popular drink around the world and contains essential minerals and trace elements for human health. In this study, the analytical capabilities of the total-reflection X-ray fluorescence method (TXRF) were considered for the analysis of tea. Different sample preparation techniques, e.g. suspension, open vessel acid digestion, and microwave acid digestion were examined. The influence of particle size was investigated in the analysis of the suspension of tea samples. Mass-absorption coefficients for the tea matrix and the critical surface density of the specimen were calculated. The data obtained explain the presence of absorption effects in the determination of P, S, Cl, and K in suspensions. The digestion procedure is chosen as an optimal sample preparation technique for the TXRF analysis of tea. Nineteen real tea samples were analyzed using TXRF. The advantages of TXRF have been presented through the comparison of results with the wavelength-dispersive X-ray fluorescence spectrometry method.

Biocompatible chitosan-zinc oxide nanocomposite based dispersive micro-solid phase extraction coupled with HPLC-UV for the determination of rosmarinic acid in the extracts of medical plants and water sample.

In the present research, a procedure was described for the recovery of rosmarinic acid (RA) from medical extract samples using chitosan­zinc oxide nanoparticles as a biocompatible nanocomposite (CS-ZnO-NC). The dispersive micro-solid phase extraction (D-µ-SPE) of RA from the medical extract samples was investigated by using the prepared biocompatible composite as a solid phase. The HPLC-UV method was used for measuring the extracted RA. The important variables (pH, biocompatible composite mass, contact time, and volume of eluent) associated with the extraction process were analyzed by the application of central composite design (CCD). The achieved optimum values for the mentioned variables were 7.0, 10 mg, 4 min, and 180 µL, respectively. The extraction recovery (99.68%) obtained from the predicted model was in agreement with the experimental data (98.22 ± 1.33%). In addition, under the obtained optimum conditions and over the concentration in the range of 2-3500 ng mL-1, a linear calibration curve was obtained with R2 > 0.993. The limit of detection (LOD) and quantification (LOQ) values were computed, and the obtained ranges were respectively from 0.060 to 0.089 ng mL-1 and 0.201 to 0.297 ng mL-1. In addition, the enrichment factors were obtained in the range of 93.7-110.5 with preconcentration factor of 83.3. Therefore, the D-µ-SPE-HPLC-UV method could be used for analyzing RA in the samples of the extracts obtained from the medical plants and water with the recovery values of the analyte in the range of 96.6%-105.4% and the precision with relative standard deviation <5.7%.

Characterization of biotin interference in 21 Vitros 5600 immunoassays and risk mitigation for patient safety at a large academic medical center.

BACKGROUND: Biotin and streptavidin are commonly used reagents in clinical immunoassays. Several cases of biotin interference with immunoassay testing for patients taking biotin supplements have been reported, yet, not all analytes and platforms susceptible to biotin interference have been characterized. The objectives of this study are to characterize biotin interference with 21 immunoassays using the Ortho Clinical Diagnostics Vitros 5600, evaluate a biotin-depletion method, and apply risk mitigation strategies for biotin interference during routine clinical testing at our institution. METHODS: Residual serum without and with increasing concentrations of exogenous biotin were used to evaluate biotin interference with 21 immunoassays using the Vitros 5600. Biotin-depletion was evaluated by comparing measured analyte concentrations in serum with and without exogenous biotin and streptavidin-microparticle pretreatment. Focused education for healthcare professionals about biotin interference was performed in February 2018. Samples with suspected biotin interference were investigated using this biotin-depletion method, and analyte testing by alternate methodology for select samples. RESULTS: Exogenous biotin in serum caused dose-dependent negative biases in 15 immunometric assays, and dose-dependent positive biases in 6 competitive immunoassays. Streptavidin-microparticle pretreatment of serum containing exogenous biotin demonstrated recoveries 100 ±â€¯15% of expected values for all 21 analytes. Physicians identified 21 samples suspicious for biotin interference over 11 months, and streptavidin-microparticle pretreatment verified 11 cases of biotin interference. CONCLUSIONS: Analytical bias caused by biotin interference is dependent on biotin concentration but independent of analyte concentration for immunometric methods using the Vitros 5600, and dependent on both biotin and analyte concentration for competitive immunoassays. Multi-disciplinary education and a lab streptavidin-microparticle pretreatment method help mitigate risk of erroneous results due to biotin interference for patient safety.

Binary code, a flexible tool for diagnostic metabolite sequencing of medicinal plants.

The principle of chromatographic fingerprint is that certain diagnostic metabolites should be always distributed in a given plant and currently, it has been widely accepted as a promising means for medicinal plant authentication. Moreover, the chemical profile is the only evidence to clarify the ingredients of those consumable plant products, e.g. traditional Chinese medicine (TCM) prescriptions. Herein, efforts were made to describe the diagnostic metabolome of medicinal plant or TCM prescription using a binary code sequence. Forty-five well-known medicinal plants along with six relevant prescriptions were employed for concept illustration and proof. Each plant was subjected to chemical characterization, and diagnostic metabolites of all plants were gathered into a chemical pool containing 595 compounds. A robust method enabling the detection of all 595 constituents was then developed using LC coupled to scheduled multiple reaction monitoring. Analyst™ software was responsible for automatically judging the presence (defined as "1") or absence (defined as "0") of each analyte with a defined signal-to-noise threshold (S/N > 100). After converting each medicinal plant to a binary sequence consisting of 595 codes, an in-house database was built by involving all sequences. The potentials of sequence library retrieval towards plant authentication, preliminary chemical characterization, and deformulation of TCM prescriptions were demonstrated after that the diagnostic metabolome of each test sample was translated to a binary code sequence. Above all, binary code is a flexible tool for diagnostic metabolite sequencing of medicinal plants, and it should be an alternative tool of DNA barcoding towards plant authentication.

Development of UPLC-Q-TOF-MS Coupled with Cation-exchange Solid-phase Extraction Method for the Determination of Ten Pyrrolizidine Alkaloids in Herbal Medicines.

Pyrrolizidine alkaloids are secondary metabolites of plants and can cause significant hepatotoxicity in humans. In this study, a fast and simple method was developed to determine ten pyrrolizidine alkaloids (PAs) in six types of herbal medicines using ultra performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS). An efficient solid-phase extraction procedure was carried out by using strong cation-exchange cartridges and the parameters were optimized. The established analytical method was validated and the results showed that the method presented satisfactory accuracy and precision. The established method was successfully applied for the determination of PAs in six herbal plants, including Senecionis Scandentis Hebra, Arnebiae Radix, Asteris Radix Et Rhizoma, Farfarae Flos, Senecionis Cannabifolii Herba and Emilia sonchifolia. PAs were found in all of these herbal plant samples. Eight types of related commercial herbal drugs were also detected, six of them were detected with different amounts of PAs. This work not only provided a powerful technical platform for both qualitative and quantitative analysis of PAs in herbal medicines, but also obtained information concerning PAs in these herbal samples, which could provide reference to the government regulatory authorities and non-governmental organizations.

The first method for determination of lipoyllysine in human urine after oral lipoic acid supplementation.

Aim: The first method on urinary excreted amounts of lipoyllysine (LLys) after lipoic acid (LA) supplementation was developed and validated. The suggested procedure allowed simultaneous determination of LLys and LA. Methodology & results: After the conversion of analytes into their reduced forms with tris(2-carboxyethyl)phosphine and derivatization via thiol group with 1-benzyl-2-chloropyridinium bromide, separation of analytes derivatives was performed on C18 column using a gradient mobile phase consisting of acetic acid and acetonitrile. The calibration curves for LA and LLys were linear (R2 > 0.999) in the range of 0.4-12 µM concentration and all validation results were acceptable, according to the US FDA bioanalytical method guidelines. Conclusion: This method was effectively applied for LA and LLys quantification in human urine after oral LA supplementation.

Recent advances of modern sample preparation techniques for traditional Chinese medicines.

Traditional Chinese medicines (TCMs) have been widely applied to the prevention and treatment of various illnesses for thousands of years. Sample preparation played a crucial role in the analysis of TCMs because of the complexity of the sample matrixes. In this paper, recent developments and applications of modern sample preparation techniques for the analysis of TCMs were summarized. The sample preparation techniques to pretreat herbal matrixes included ultrasound-assisted extraction, microwave-assisted extraction, pressurized-liquid extraction, supercritical-fluid extraction, synergistic extraction techniques and so on. The sample preparation techniques mainly applied to pretreating biological matrixes such as microdialysis and microfluidic technique were presented. The sample preparation techniques applied to both herbal and biological matrixes were discussed as well, involving solid phase extraction, matrix solid phase dispersion, solid phase microextraction, cloud point extraction, online coupling sample preparation techniques and so on. In addition, the trends for sample preparation techniques of TCMs were proposed.

Natural deep eutectic solvents for sample preparation prior to elemental analysis by plasma-based techniques.

Natural deep eutectic solvents (NADES) based on xylitol, citric acid, and malic acid were synthesized and were then characterized using infrared spectroscopy, thermogravimetry (TG), differential scanning calorimetry (DSC), also density and viscosity were measurements. The deep eutectic solvents were used as solvent in ultrasound-assisted extraction (DES-UAE) of plant samples prior to elemental analysis. Inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-optical emission spectrometry (ICP OES) were employed for the determination of As, Ca, Cd, Cu, Fe, K, Mg, Mn, Na, P, and Zn in the extracts. The infrared analyses of the NADES revealed bands characteristic of the initial reagents, with the presence of hydrogen bonds, which confirmed the formation of a NADES. The thermal analyses showed decomposition temperatures of around 170 °C and endothermic events related to degradation of the NADES. The viscosity and density parameters were found to be related to the presence of hydrogen bonds. The extraction recoveries ranged from 80% to 120%, with some analytes presenting poor recoveries. There were no significant differences between the NADES, in terms of the concentrations of the analytes found in the extracts. However, there were differences between the analyte concentrations obtained using the NADES extraction method and the concentrations obtained using microwave-assisted acid digestion (MW-AD), possibly due to the different types of interactions between the solvents and the analytes. Plant tissues are complex matrices containing substantial amounts of silica, so some elements may be tightly bound and consequently difficult to release. The results indicated that UAE using NADES is a promising technique for the elemental extraction of plant samples.

Plant Metabolomics: Evaluation of Different Extraction Parameters for Nontargeted UPLC-ESI-QTOF-Mass Spectrometry at the Example of White Asparagus officinalis.

The extraction of metabolites turns out to be one of the most important key factors for nontargeted metabolomics approaches as this step can significantly affects the informative value of the successive measurements. Compared to metabolomics experiments of various matrices of bacterial or mammalian origins, there are only few studies, which focus on different extraction methods for plant metabolomics analyses. In this study, various solvent extraction compositions were compared and assessed using an UPLC-ESI-QTOF-MS strategy. Exemplary, white asparagus ( Asparagus officinalis) were employed as a low-fat-, low-protein-, high-water-content model commodity with the objective of designing an optimal nontargeted extraction protocol for polar and nonpolar metabolites. Furthermore, the influence of acid addition, mechanical cell disruption methods (ball mill, ultrasonic bath, vortex mixer), and extract stability have been systematically scrutinized too. The different extraction protocols were compared based on sum of features, sum of peak intensities, sum of peak areas, as well as by analyzing individual signals of as many different substance groups as possible to obtain a maximum overview.

A novel strategy to evaluate the quality of herbal products based on the chemical profiling, efficacy evaluation and pharmacokinetics.

The purpose of this study was to establish a chemical profiling method to compare the chemical composition of herbal products by using extracts of Belamcandae Rhizoma(EBR) extracted with different polarity solvent as an example, and evaluate the quality of EBR based on the analysis of chemical profiling, efficacy evaluation and pharmacokinetics. As seen from the results of chemical profiling, the PCA and PLS-DA score plot indicated that the dots of Belamcandae Rhizoma water extracts were separated from ethanol extracts obviously, which suggested significant differences of chemical profiling existing in the different solvent extracts. The PCA and PLS-DA loading plot illustrated that the main compounds contributing to chemical profiling differences were tectoridin(TD), iristectorin B(IT B), iridin(ID), tectorigenin(TG), irigenin(IG), iristectorigein A(IG A), dichotomitin(DT) and irisflorentin(IF). Furthermore, the results of HPLC analysis demonstrated that the contents of these main compounds in ethanol extracts were significantly higher than that in water extracts (P < 0.01). Both the pharmacological and hematoxylin-eosin staining studies indicated that the ethanol extracts of Belamcandae Rhizoma had a better therapeutic effect than water extracts in oral ulcer model rats (P<0.01). It is suggested that the ethanol extracts were beneficial to the absorption and bioavailability of TG which was one of the most important bioactive compounds of Belamcandae Rhizoma in pharmacokinetic study in rats. This work provided a novel method to optimize the extraction process of EBR and related herbal products. Compared with the conventional chemical fingerprint methodology, the approach proposed above is not only a powerful tool to identify efficacy-related components for the quality evaluation, but also can be used to predict the therapeutic efficacy of herbal products.

Advancement in the chemical analysis of Paeoniae Radix (Shaoyao).

Paeoniae Radix Alba (baishao or white peony root) and Paeoniae Radix Rubra (chishao or red peony root) are two highly valuable traditional Chinese medicines (TCMs) usually indicated for painful conditions, menstrual disorders and viral infections. These two TCMs are collectively referred to as shaoyao (Paeoniae Radix) due to their close origins and similar chemical compositions. Modern research indicates that monoterpene glycosides, polyphenols and paeonols are the three main types of compounds related to the pharmacological activities of Paeoniae Radix. This review summarizes recent advances in the chemical analysis of Paeoniae Radix and the related traditional Chinese medicine formulas/preparations, including methods used for sample pretreatment, qualitative analysis, quantitative analysis and biological sample analysis. More than 120 papers are discussed in this review, focusing on the chemical analysis of Paeoniae Radix, and various analytical techniques (such as HPLC, LC-MS, IR, near IR and quantitative NMR), as well as their advantages/disadvantages, are described. It is our hope that this paper can provide necessary information for improving the quality evaluation methods currently available for Paeoniae Radix and offer a scientific basis for the future in-depth study of the pharmacokinetics and pharmacodynamics of Paeoniae Radix.

Validated UPLC-MS/MS method for the quantification of dasatinib in plasma: Application to pharmacokinetic interaction studies with nutraceuticals in Wistar rats.

Dasatinib (DAS) is a tyrosine kinase inhibitor (TKI) used in the treatment of chronic myeloid leukemia and in the management of ulcerative colitis (UC). Since some nutraceuticals (e.g. curcumin, olive oil, and cocoa extract) could alter the function of ABC transporters and /or CYP450 enzymes, DAS bioavailability could potentially be affected following their co-administration. This work aims at studying the possibility of PK interaction between DAS and the selected nutraceuticals in UC rats using UPLC- MS/MS. Chromatographic analysis was carried out using BEH C 18 column (Waters) with a mobile phase consisting of acetonitrile and 50% aqueous methanol, 65:35, v/v, each with 0.1% formic acid and using erlotinib (ERL) as an internal standard (IS). DAS quantitation was carried out using multiple reaction monitoring (MRM) with positive ionization of the transitions at m/z 488.03 > 400.92 (DAS), and m/z 394.29 > 278.19 (ERL). Method validation was assessed as per the FDA guidelines for bioanalytical methods for DAS determination within the concentration range 1-500 ng/mL. No significant effect on the oral bioavailability of DAS was reported with any of the studied nutraceuticals. Thus, the concomitant administration of these nutraceuticals with DAS could be considered safe with a necessity to perform more detailed clinical investigations.

A second-derivate fitting algorithm for the quantification of free hemoglobin in human plasma.

BACKGROUND: Assessment of hemolysis in vivo is becoming increasingly relevant in critical care. Current methods (Harboe, 1959) for quantifying the free hemoglobin (fHb) content produce unsatisfactory results in case of hyperbilirubinemia, a frequent condition in patients at risk for intravascular hemolysis. METHODS: A novel evaluation method based on second-derivative fitting to quantify fHb content was developed. The method uses spectrophotometric data from 350 to 650 nm recorded with standard instruments as input. To evaluate the power of the new method, plasma of patients and non-icteric plasma of healthy volunteers were spiked with fHb concentrations up to 2000 mg/L and compared to methods described in the literature by Harboe, Noe and Fairbanks. All measurements were done in compliance with the bioanalytical method validation protocol from the European Medicines Agency. RESULTS: Both the second-derivative fitting algorithm as well as the methods of Harboe, Noe and Fairbanks quantified fHb accurately in non-icteric samples, with inaccuracy and imprecision below 10%. For icteric specimen, false high results were obtained with the established formulas for fHb concentrations below 700 mg/L. In contrast, no interference was found with the second-derivate fitting method for bilirubin concentrations up to 465 µmol/L. The lower limits of quantifications for the second-derivative fitting algorithm were specified in agreement with the EMA guideline with 25 mg/L fHb for both non-icteric and icteric specimens. CONCLUSIONS: A user-friendly, computer-based algorithm is reported that allows the accurate quantification of fHb concentrations in the presence of high bilirubin concentrations. The new method allows for uniform sample preparation with only a single dilution step and can be readily implemented in any laboratory on standard spectrophotometers using the provided supplementary Microsoft Excel macro.

Aflatoxins in sunflower seeds and unrefined sunflower oils from Singida, Tanzania.

A total of 61 samples comprising sunflower seeds (40) and unrefined sunflower oils (21) samples collected randomly from Singida, Tanzania were analysed by Reverse Phase-high performance liquid chromatography (RP-HPLC). 15% (6/40) of the seed samples were contaminated with aflatoxin B1 ranging from limit of detection (LOD) to 218 ng g-1 with three of them exceeding the European Commission/European Union (EC/EU) and Tanzania Bureau of Standards (TBS)/Tanzania Food and Drug Authority (TFDA) maximum limits of 2 ng g-1 for AFB1 in oilseeds. The levels of total aflatoxins (AFT) in seeds ranged from LOD to 243 ng g-1. Other aflatoxins, except AFG2, were also detected. For the unrefined sunflower oils, the levels of AFB1 ranged from LOD to 2.56 ng mL-1. About 80.9% (17/21) of the analysed oil samples contained AFB1 of which 17.65% (3/17) exceeded the EC/EU and TBS/TFDA maximum limits of 2 ng mL-1. Other aflatoxins were also detected in the oils. The measured levels indicate there is a need for food quality education among food processors.

Polycyclic aromatic hydrocarbons in teas using QuEChERS and HPLC-FLD.

Polycyclic aromatic hydrocarbons (PAHs) are food-processing contaminants considered to be carcinogenic and genotoxic. Due to its drying process stage, teas may be contaminated with PAHs. The aim of the study was to validate an analytical method involving QuEChERS and HPLC-FLD for the determination of PAH4 in teas and evaluate the contamination levels in 10 different types of teas from Brazil. Recoveries varied from 54% to 99% and relative standard deviations from 1% to 21%. Limits of detection and quantification were from 0.03 to 0.3 µg/kg and 0.1 to 0.5 µg/kg, respectively. Mate tea presented the highest PAH levels, with PAH4 varying from 194 to 1795 µg/kg; followed by black (1.8-186 µg/kg), white (24-119 µg/kg), and green teas (3.1-92 µg/kg). Teas with lowest PAH4 were strawberry, lemongrass, peppermint, and boldo. Only trace levels of PAHs were detected in tea infusions, so apparently it would not affect PAH intake by Brazilian population.

A simple in chemico method for testing skin sensitizing potential of chemicals using small endogenous molecules.

Among many of the validated methods for testing skin sensitization, direct peptide reactivity assay (DPRA) employs no cells or animals. Although no immune cells are involved in this assay, it reliably predicts the skin sensitization potential of a chemical in chemico. Herein, a new method was developed using endogenous small-molecular-weight compounds, cysteamine and glutathione, rather than synthetic peptides, to differentiate skin sensitizers from non-sensitizers with an accuracy as high as DPRA. The percent depletion of cysteamine and glutathione by test chemicals was measured by an HPLC equipped with a PDA detector. To detect small-size molecules, such as cysteamine and glutathione, a derivatization by 4-(4-dimethylaminophenylazo) benzenesulfonyl chloride (DABS-Cl) was employed prior to the HPLC analysis. Following test method optimization, a cut-off criterion of 7.14% depletion was applied to differentiate skin sensitizers from non-sensitizers in combination of the ratio of 1:25 for cysteamine:test chemical with 1:50 for glutathione:test chemical for the best predictivity among various single or combination conditions. Although overlapping HPLC peaks could not be fully resolved for some test chemicals, high levels of sensitivity (100.0%), specificity (81.8%), and accuracy (93.3%) were obtained for 30 chemicals tested, which were comparable or better than those achieved with DPRA.

Critical Assessment of Analytical Techniques in the Search for Biomarkers on Mars: A Mummified Microbial Mat from Antarctica as a Best-Case Scenario.

The search for biomarkers of present or past life is one of the major challenges for in situ planetary exploration. Multiple constraints limit the performance and sensitivity of remote in situ instrumentation. In addition, the structure, chemical, and mineralogical composition of the sample may complicate the analysis and interpretation of the results. The aim of this work is to highlight the main constraints, performance, and complementarity of several techniques that have already been implemented or are planned to be implemented on Mars for detection of organic and molecular biomarkers on a best-case sample scenario. We analyzed a 1000-year-old desiccated and mummified microbial mat from Antarctica by Raman and IR (infrared) spectroscopies (near- and mid-IR), thermogravimetry (TG), differential thermal analysis, mass spectrometry (MS), and immunological detection with a life detector chip. In spite of the high organic content (ca. 20% wt/wt) of the sample, the Raman spectra only showed the characteristic spectral peaks of the remaining beta-carotene biomarker and faint peaks of phyllosilicates over a strong fluorescence background. IR spectra complemented the mineralogical information from Raman spectra and showed the main molecular vibrations of the humic acid functional groups. The TG-MS system showed the release of several volatile compounds attributed to biopolymers. An antibody microarray for detecting cyanobacteria (CYANOCHIP) detected biomarkers from Chroococcales, Nostocales, and Oscillatoriales orders. The results highlight limitations of each technique and suggest the necessity of complementary approaches in the search for biomarkers because some analytical techniques might be impaired by sample composition, presentation, or processing. Key Words: Planetary exploration-Life detection-Microbial mat-Life detector chip-Thermogravimetry-Raman spectroscopy-NIR-DRIFTS. Astrobiology 17, 984-996.

Investigation of 1-Dodecylimidazolium Modified Filter Papers as a Thin-Film Microextraction Phase for the Preconcentration of Bisphenol A from Plant Oil Samples.

Based on the tunability of ionic liquids (ILs) according to the specific requirement of an application, 1-dodecylimidazolium chloride with amphiphilic structures was chemically fabricated on the surface of filter papers (DIL-FPs) for the first time. After synthesis, DIL-FPs was characterized by scanning electronic microscopy, energy dispersive X-ray spectroscopy and Fourier-transform infrared spectroscopy. DIL-FPs was used as a novel thin-film microextraction (TFME) phase for the preconcentration of amphiphilic bisphenol A from plant oil samples. The related extraction variables were studied in a spiked sunflower seed oil. Under the optimal conditions, the linear range was 5.0 - 1000 µg L-1 with a correlation coefficient of 0.9976. The limit of detection (S/N = 3) and the enrichment factor of the proposed method were 2.7 µg L-1 and 118, respectively. The intra-day precision and inter-day precision for six repeated determinations were 2.3 and 4.9%, respectively. These plant oil samples used in this work were free of bisphenol A contaminations. The recovery study carried out in different plant oil samples and mean recoveries ranged from 77.16 to 97.10%. The developed DIL-FPs extraction film phase followed by HPLC-UV provides a potential pretreatment strategy for the analysis of weak organic acid compounds in plant oil samples.

Aflatoxin B1 in sesame seeds and sesame products from the Greek market.

Aflatoxin B1 (AFB1) is considered as the most potent liver carcinogen for humans. A method for determination in sesame seeds was developed. AFB1 was extracted by methanol-water, cleaned by immunoaffinity columns and determined by high-performance liquid chromatography with fluorescence detection. The recovery factor and the limit of detection (LOD) of AFB1 in sesame seeds were 111.5% and 0.02 ng g(-1), respectively. Thirty samples of sesame products were examined for the presence of AFB1. After analysis, 77.6% of samples were found to be contaminated. Eight samples exceeded the European Union (EU) limit (2 µg AFB1 kg(-1)). In 15 samples, AFB1 was below the EU limit. Seven samples remained below the LOD. The most contaminated (14.49 ng AFB1 g(-1)) sample was unpeeled packaged sesame seeds. In all samples, aflatoxigenic Aspergilli fungi as well as the risk for AFB1 presence in sesame seed was investigated.