Liquid Chromatography-triple Quadrupole Mass Spectrometry Research Articles

Construction of Fe3O4/SiO2/chitosan-grafted-poly(N-vinylcaprolactam) magnetic nanocomposite and their application in simultaneous extraction of Trans-resveratrol and its metabolites from rat plasma

A novel magnetic nanocomposite of chitosan-grafted-poly(N-vinylcaprolactam) (Fe3O4/SiO2/CHT-g-PNVCL MNC) were synthesized. Chitosan was prepared from shrimp shells Penaeus monodon by a green deacetylation approach. N-vinylcaprolactam was first polymerized on the surface of Fe3O4 magnetic nanoparticles using surface-initiated atom transfer radical polymerization. Then, the Fe3O4 nanoparticles modified with carboxyl-terminated- poly(N-vinylcaprolactam) was grafted onto chitosan. Various techniques were used to characterize of physicochemical properties of synthesized nanomaterials. The application of Fe3O4/SiO2/CHT-g-PNVCL MNC was utilized as a novel adsorbent for the simultaneous extraction of trans-resveratrol and its major phase II metabolites from rat plasma. A qualitative analysis was performed using ultra-performance liquid chromatography triple-quadrupole tandem mass spectrometry. Response surface methodology based on central composite design was used to optimize the extraction procedure including pH, amount of adsorbent, extraction time, desorption time, and volume of elution solvent. The established quantitative method succeeded in satisfying FDA requirements regarding biological analysis methods. The results of the validation of the method indicated its acceptable accuracy (−4.4 to 6.9%), linearity (r > 0.995), precision (CV < 6.3%), and stability. The lower limits of quantification of the proposed method achieved were 1.23–1.68 ngmL−1for target analytes. The information obtained from the method validation has been used to estimate the expanded uncertainty for the determination of trans-resveratrol in rat plasma samples following orally administered trans-resveratrol. The method was applied to study the pharmacokinetics, metabolism, and bioavailability of trans-resveratrol in healthy rats following a single oral or intravenous dose.

Simultaneous determination of 14 pesticide residues in tea by multi-plug filtration cleanup combined with LC-MS/MS

A combined method of multi-plug filtration cleanup (m-PFC) and liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was established to simultaneously detect 14 pesticides in tea. The pesticides in water-soaked tea were extracted with acetonitrile. Cleanup of tea extract was performed using an m-PFC column packed with multiple cleanup materials: multi-walled carbon nano-tubes (MWCNTs), primary secondary amine (PSA) and anhydrous magnesium sulfate (MgSO4). The cleanup effect of the column was evaluated based on the rates of removal of tea components that interfered with pesticide recovery, henceforth referred to as interference components. Results showed that 14 pesticides had strong linearity in the range of 5–500 μg L−1 (r2 > 0.99). The quantitative limits were within the range of 3–50 μg kg−1. The average recoveries of 14 pesticides spiked into three different blank tea samples (green tea, black tea, oolong tea) at three levels of 0.05, 0.50 and 2.00 mg kg−1 were in the range of 62.3–108.8% with relative standard deviations of 0.2–13.6%. The m-PFC method can greatly improve the efficiency of sample pretreatment. Furthermore, this work provides methodological guidance on how to select cleanup materials and allocate their proportions.

Association between Pre-Diagnostic Serum Bile Acids and Hepatocellular Carcinoma: The Singapore Chinese Health Study.

Simple SummaryHepatocellular carcinoma (HCC) is a common cancer with poor prognosis. The increasing incidence rate of HCC in developed countries has been linked to increasing prevalence of metabolic dysfunction-associated fatty liver disease, which has characteristics of altered bile acid metabolism that may predate hepatocarcinogenesis. The aim of the present study was to assess the association of circulating bile acid levels in pre-diagnostic serum with the risk of developing HCC in a general population in Singapore. Primary conjugated bile acids were most strongly associated with increased risk of HCC whereas the ratios of secondary over primary bile acids were significantly associated with reduced risk. These results support a contributing role of dysmetabolism of bile acids in the development of HCC. The modulation of bile acid metabolism through alteration of gut microbiota may be an effective strategy for primary prevention against HCC in individuals with metabolic dysfunction-associated fatty liver disease.Hepatocellular carcinoma (HCC) is a commonly diagnosed malignancy with poor prognosis. Rising incidence of HCC may be due to rising prevalence of metabolic dysfunction-associated fatty liver disease, where altered bile acid metabolism may be implicated in HCC development. Thirty-five bile acids were quantified using ultra-performance liquid chromatography triple-quadrupole mass spectrometry assays in pre-diagnostic serum of 100 HCC cases and 100 matched controls from the Singapore Chinese Health Study. Conditional logistic regression was used to assess associations for bile acid levels with risk of HCC. Conjugated primary bile acids were significantly elevated whereas the ratios of secondary bile acids over primary bile acids were significantly lower in HCC cases than controls. The respective odds ratios and 95% confidence intervals of HCC were 6.09 (1.75–21.21) for highest vs. lowest tertile of cholic acid species and 30.11 (5.88–154.31) for chenodeoxycholic acid species. Doubling ratio of taurine-over glycine-conjugated chenodeoxycholic acid was associated significantly with 40% increased risk of HCC whereas doubling ratio of secondary over primary bile acid species was associated with 30–40% reduced risk of HCC. In conclusion, elevated primary bile acids and taurine over glycine-conjugated ratios were strongly associated with HCC risk whereas the ratios of secondary bile acids over primary bile acids were inversely associated with HCC risk.

Variations in phenolic acids and antioxidant activity of navel orange at different growth stages

Ripe navel orange has abundant amounts of phenolic compounds. Few studies monitored changes in these compounds during ripening. In this study, the effects of navel orange maturation on dynamic changes in antioxidant activity, total phenolic content (TPC), total flavonoid content (TFC) and phenolic acids were investigated. Five growth stages of navel orange were studied, and nine phenolic acids were detected via high performance liquid chromatography–triple quadrupole mass spectrometry (HPLC–QQQ–MS). Results showed that antioxidant activity, TFC and TPC decreased gradually with fruit ripening. The concentrations of most phenolic acids also declined during fruit maturation, except for free fractions of sinapic acid and bound fractions of ferulic and caffeic acids. Ferulic acid was the most dominant of all phenolic acids at all growth stages. Partial least-squares showed significant differences among fruits of different maturities. A significant correlation between antioxidant capacity, TPC, TFC and some phenolic acids was found.

Analysis of synthetic antioxidants in salmon silage using QuEChERS extraction method followed by determination by LC-MS/MS; a single-laboratory validation study

A new method was developed and in-house validated to determined ethoxyquin (EQ), butylated hydroxyanisole (BHA) and propyl gallate (PG) in fish silage and fish oil used for production of animal feed. Sample pre-treatment comprises use of QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction and gives extracts for liquid chromatography-triple quadrupole mass spectrometry analysis without matrix interferences. The results allow quantification of the antioxidants in all matrices by using deuterated internal standards and calibration curves made in solvent, as well as establishing low detection limits (0.012–0.015 mg/kg) and quantification limits (0.040–0.050 mg/kg) needed regarding the recent suspension of EQ as feed additive within the European Union. The proposed method was validated in terms of linearity, accuracy (relative error, ±1.4%), precision (RSD, ≤2.7%) and recovery (matrix effect, 97–101%) where all the parameters show acceptable results according to recognized guidelines (including EuraChem) within method validation. Combined expanded measurement uncertainty was estimated with a coverage factor of 2 by including all contributors to analytical variation, showing results of ±15% or better. The combined QuEChERS and LC-MS/MS method was successfully applied to salmon silage samples and their corresponding aqueous and oil fractions.

Determination of caffeine content in Ginkgo Folium by ultra high performance liquid chromatography-triple quadrupole mass spectrometry

In this experiment, an ultra-high performance liquid chromatographytandem triple quadrupole mass spectrometry was established for the determination of caffeine in commercially available Ginkgo Folium. The samples were extracted by ultrasonic method with methanol, and separated on Waters CORTECS T3 column(2.1 mm×100 mm, 2.7 μm), with mobile phase of 0.1% formic acid solution-0.1% formic acid acetonitrile solution for gradient elution, at flow rate of 0.3 mL·min~(-1); column temperature of 30 ℃, and injection volume of 2 μL. Mass spectrometry was conducted at ESI~+ multiple reaction monitoring(MRM) mode; quantitative analysis was conducted with external standard method. The results showed that in the range of 0.099 6-9.96 ng·mL~(-1), there was a good linear relationship between the mass concentration of caffeine and the peak area, R~2=0.999; the average recovery was 84.51%, with RSD of 6.2%. The results of precision, repeatability and stability showed that the RSD was 5.1%, 5.9%, 7.2%, respectively. The content range of caffeine in 10 batches of Ginkgo Folium was 1.52-60.86 μg·kg~(-1). In conclusion, this method is accurate, reliable and reproducible, which provides a reference for the safety study of Ginkgo Folium.

DIAGNOSTIC ACCURACY OF DRUG SCREENING IMMUNOASSAYS IN DRUG FACILITATED CRIMES

Objective: To determine the diagnostic accuracy of immunoassays in drug screening as required in emergency for the rapid diagnosis of drug intoxication in travel related crimes.&#x0D; Study Design: Diagnostic accuracy study.&#x0D; Place and Duration of Study: department of Chemical Pathology and Endocrinology, Armed Forces Institute ofPathology, Rawalpindi Pakistan, from Jul 2017 to Jun 2018.&#x0D; Methodology: Sealed urine specimens of 77 patients with history of suspected intoxication in drugs facilitatedstreet crimes, received for toxicology screening were included in the study. All the specimens were analysed,initially on immunoassay (index test) and then on Triple Quadrupole Liquid chromatography–Mass spectrometry (reference standard). Benzodiazepine being the main class of drugs involved in travel related crimes, diagnostic accuracy of immunoassay technique was assessed for these by calculating its sensitivity, specificity, positive predictive value and negative predictive value.&#x0D; Results: Victims were predominantly males and public transportation was the most common mode of transport. The most commonly used drug was Lorazepam. Immunoassay failed to detect few cases who were shown to be intoxicated with benzodiazepines by liquid-chromatography tandem mass spectrometry. The false negative rate was 4.9%. Only one false positive case was observed. The accuracy was calculated to be 94.8% with sensitivity of 95.08% and specificity of 93.7%.&#x0D; Conclusion: Immunoassay was found reliable for rapid testing in drug facilitated intoxication cases. Howevercritical decision making should be done cautiously keeping in mind the limitations associated with thesescreening procedures.

Validation of Quick Polar Pesticides (QuPPe) Method for Determination of Eight Polar Pesticides in Cherries by LC-MS/MS

A novel and sensitive chromatography method with modified Quick Polar Pesticide (QuPPe) sample preparation was validated for determination of eight high polar pesticides in cherries by liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS). The validation data executed the conditions of the European SANTE/12682/2019 Guidance Document. Good linearity (R2 > 0.99) was observed, and the residuals were lower than ± 20%. Average recoveries ranged from 70.2 to 105.1%, and LOQ values ranged from 1.77 to 12.13 μg kg−1. The repeatability and reproducibility are in range of 1.57–15.56% and 3.51–16.17% separately. All measurement uncertainty values were lower than 50% for all polar pesticides. This verified analytical method was used to detect pesticide residue levels of cherries, and none of the eight high polar pesticides were found in 225 real samples. This is the first validation report of QuPPe sample preparation and LC-MS/MS method of high polar pesticide residues in cherries from Turkey.

Screening of hypolipidemic active components in Jiang-Zhi-Ning and its preliminary mechanism research based on “active contribution value” study

Ethnopharmacological relevanceJiang-Zhi-Ning (JZN) is a traditional Chinese medicine formula, which has the effect of lowering blood lipid level and softening blood vessels. It is clinically used in the treatment of hyperlipidemia with significant curative effect. Aim of the studyThis study aims to screen the active components of JZN that are responsible for its blood lipids lowering effect and lay the foundation for elucidating pharmacodynamic material basis of the hypolipidemic effect of the formula. Materials and methodsThe hyperlipidemia model was used to evaluate the efficacy of the JZN effective extraction with the TC and TG of rat plasma as evaluation index. Then the established ultra-high performance liquid chromatography coupled with electrospray ionization-quadrupole-time of flight-mass spectrometry (UPLC-ESI-Q-TOF-MSn) method was utilized to analyze the components of JZN effective extraction and the absorbed components in rat plasma, the potential active components were screened by using the combined analysis results of in vivo and in vitro component identification. Then an established ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QqQ-MSn) method was used to determine the content of potential active components and its natural ratio in JZN effective extraction, and a potential active components combination (PACC) was formed accordingly. Then a HepG2 cell hyperlipidemia model induced by sodium oleate was used to study the hypolipidemic activity of PACC by detecting the content of TG level in the model. Meanwhile, the real-time quantitative reverse transcription polymerase chain reaction (qRT-PCR) was used to conduct preliminary research on its hypolipidemic mechanism. Then combined with the concept of “combination index” in the “median-effect principle”, to calculate the half inhibitory concentration (IC50) values of PACC and each monomer component on inhibiting the TG level in the cell model. Subsequently, the “activity contribution study” was carried out, and the components with the sum of the “activity contribution value” of 85% were finally selected as the hypolipidemic active components of JZN. ResultsThe pharmacodynamics results showed that JZN effective extraction has displayed a good hypolipidemic effect. 45 components were identified in vitro, 108 components were identified from rat plasma, and 17 potential active components were screened out. The content determination result showed that the ratio of each potential active components in PACC as following: cassiaside C: rubrofusarin-6-O-gentiobioside: aurantio-obtusin-6-O-glucoside: hyperoside: isoquercitrin: quercetin-3-O-glucuronide: (E)-2,3,5,4′-tetrahydroxystilbene-2-O-glucoside: rutin: emodin-8-O-glucoside: astragalin: armepavine: N-nornuciferine: coclaurine: O-nornuciferine: nuciferine: N-norarmepavine: higenamine = 3.30: 16.06: 9.15: 23.94: 98.40: 417.45: 189.68: 8.62: 1.28: 5: 3.51: 14.57: 1.06: 1.35: 1: 5.64: 6.06, and the activity study results showed that it has displayed a good hypolipidemic activity. Finally, the hypolipidemic active components screened out by the “activity contribution study” were: quercetin-3-O-glucuronide, (E)-2,3,5,4′-tetrahydroxystilbene-2-O-glucoside, isoquercitrin, O-nornuciferine, hyperoside and rubrofusarin-6-O-gentiobioside. ConclusionsA scientific and rational approach of screening the hypolipidemic active ingredients of JZN has been developed in the current study. In addition, the research revealed the blood lipid lowering mechanism of those ingredients, which provide a solid basis for further elucidating the hypolipidemic pharmacodynamic material basis and action mechanism of JZN.

Determination of Polyphenols in Ilex kudingcha and Insect Tea (Leaves Altered by Animals) by Ultra-high-performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry (UHPLC-QqQ-MS) and Comparison of Their Anti-Aging Effects.

Ilex kudingcha C.J. Tseng tea and insect tea, as traditional Chinese teas, are favored for their original craftsmanship, unique flavor, and biological functionality. In this study, ultra high-performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-QqQ-MS) was used to analyze the bioactive components of the extracts of Ilex kudingcha and insect tea, and D-galactose-induced aging mice were used to compare the in vivo anti-aging effects of Ilex kudingcha and insect tea extracts. The results were remarkable, UHPLC-QqQ-MS analysis showed that ITP contains 29 ingredients, while IKDCP contains 26 ingredients. However, due to the large differences in the content of the main chemical components in IKDCP and ITP, the effects are equally different. At the same time, the in vivo research results suggesting that the anti-aging effects of IKDCP and ITP (500 mg/kg) include the regulation of viscera indices of major organs; improvement in liver, skin, and spleen tissue morphology; decreased production of inflammatory cytokines; up regulation of SOD, CAT, GSH, GSH-PX, and T-AOC and down regulation of NO and MDA levels in serum and liver tissue; reductions in the concentration of pro-inflammatory factors, and increases in the concentration of anti-inflammatory factor. RT-qPCR and western blot assay also showed that IKDCP and ITP affect anti-aging by regulating the gene and protein expression of GSH-PX, GSH1, SOD1, SOD2, and CAT. The overall results indicate that ITP is more effective in treating oxidative damage in aging mice induced by D-galactose. Thus, ITP appears to be an effective functional drink owing to its rich nutritional components and anti-aging activities.

A QuEChERS-HPLC-MS/MS Method with Matrix Matching Calibration Strategy for Determination of Imidacloprid and Its Metabolites in Procambarus clarkii (Crayfish) Tissues.

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues.

Terahertz Spectroscopy for Accurate Identification of Panax quinquefolium Basing on Nonconjugated 24(R)-Pseudoginsenoside F11.

Panax quinquefolium is a perennial herbaceous plant that contains many beneficial ginsenosides with diverse pharmacological effects. 24(R)-pseudoginsenoside F11 is specific to P. quinquefolium, a useful biomarker for distinguishing this species from other related plants. However, because of its nonconjugated property and the complexity of existing detection methods, this biomarker cannot be used as the identification standard. We herein present a stable 24(R)-pseudoginsenoside F11 fingerprint spectrum in the terahertz band, thereby proving that F11 can be detected and quantitatively analyzed via terahertz spectroscopy. We also analyzed the sample by high-performance liquid chromatography-triple quadrupole mass spectrometry. The difference between the normalized data for the two analytical methods was less than 5%. Furthermore, P. quinquefolium from different areas and other substances can be clearly distinguished based on these terahertz spectra with a standard principal component analysis. Our method is a fast, simple, and cost-effective approach for identifying and quantitatively analyzing P. quinquefolium.

Irrigation of wheat with select hydraulic fracturing chemicals: Evaluating plant uptake and growth impacts.

Oilfield flowback and produced water (FPW) is a waste stream that may offer an alternative source of water for multiple beneficial uses. One practice gaining interest in several semi-arid states is the reuse of FPW for agricultural irrigation. However, it is unknown if the reuse of FPW on edible crops could increase health risks from ingestion of exposed food, or impact crop growth. A greenhouse experiment was conducted using wheat (Triticum aestivum) to investigate the uptake potential of select hydraulic fracturing additives known to be associated with health risks. The selected chemicals included acrylamide, didecyldimethylammonium chloride (DDAC), diethanolamine, and tetramethylammonium chloride (TMAC). Mature wheat grain was extracted and analyzed by liquid chromatography-triple quadrupole mass spectrometry (LC-QQQ) to quantify chemical uptake. Plant development observations were also documented to evaluate impacts of the chemicals on crop yield. Analytical results indicated that TMAC and diethanolamine had significantly higher uptake into both wheat grain and stems than control plants which were not exposed to the four chemicals under investigation. Acrylamide was measured in statistically higher concentrations in the stems only, while DDAC was not detected in grain or stems. Growth impacts included lodging in treated wheat plants due to increased stem height and grain weight, potentially resulting from increased nitrogen application. While analytical results show that uptake of select hydraulic fracturing chemicals in wheat grain and stems is measurable, reuse of FPW for irrigation in real world scenarios would likely result in less uptake because water would be subject to natural degradation, and often treatment and dilution practices. Nonetheless, based on the outstanding data gaps associated with this research topic, chemical specific treatment and regulatory safeguards are still recommended.

Determination of carbendazim residues in Procambarus clarkii by high performance liquid chromatography-triple quadrupole mass spectrometry

A novel method based on high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS) was established for the determination of carbendazim in Procambarus clarkii. The sample was extracted by ethyl acetate under alkaline conditions and centrifuged. The supernatant was concentrated by rotary evaporation, redissolved, and then enriched and purified on a mixed-mode cation exchange solid phase extraction column (MCX). A C18 column was used with acetonitrile and water as mobile phases in a gradient elution. Ionization was performed using an electrospray positive ion source (ESI+), and detection was achieved by MS/MS in multiple reaction monitoring (MRM) mode. The linearity for carbendazim was good in the range of 0.5-50.0 μg/L; the linear equation was y=0.19988x+0.01842; and the correlation coefficient (r2) was 0.9985. The limit of detection (LOD) and limit of quantification (LOQ) were 0.25 μg/kg and 0.50 μg/kg, respectively. At spiked levels of 0.5, 1.0, 5.0, and 50.0 μg/kg, the recoveries ranged from 83.9% to 105.5%, and the relative standard deviation ranged from 1.1% to 3.2%. This method is simple and effective for the determination of carbendazim residues in P. clarkii.

Metabolomics analysis delineates the therapeutic effects of Huangqi decoction and astragalosides on α-naphthylisothiocyanate (ANIT) -induced cholestasis in rats

Ethnopharmacological relevanceCholestasis caused by bile secretion and excretion disorders is a serious manifestation of liver disease. With limited treatment methods, it affects millions of people worldwide. Huangqi decoction (HQD), an effective traditional Chinese medicine, is used to treat chronic cholestatic liver diseases. However, the action mechanisms of it were not fully elucidated. Aim of the studyWe aim to investigate the therapeutic effect of HQD, and its active component, astragalosides, against α-naphthylisothiocyanate (ANIT)-induced cholestasis in rats based on targeted metabolomics analysis and revel the potential mechanism. Materials and methodsThe therapeutic effect of HQD and astragalosides on ANIT-induced cholestasis model rats were evaluated by serum biochemical analysis. Liver damage was identified by histopathology. The levels of bile acids (BAs) and free fatty acids (FFAs) in serum and liver tissues were measured by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-TQMS). qRT-PCR and Western blot analysis were used to measure the expression of nuclear hormone receptor, membrane receptor and BA transporter protein in cholestatic rats before and after HQD and astragalosides treatment. ResultsThe obtained data showed that the administration of ANIT caused obvious cholestasis with significantly increased intrahepatic retention of hydrophobic BAs and altered FFAs, which were consistent with the liver histopathological and serum biochemical findings. HQD and astragalosides treatment were able to attenuate ANIT-induced BAs and FFAs perturbation, ameliorate the impaired liver function, histopathological ductular reaction, and lipid peroxidation damage by ANIT. Elevated mRNA and protein expression of transporters related to BA metabolism and genes related to lipogenesis and lipid oxidation metabolism in cholestasis were attenuated or normalized by HQD and astragalosides treatment. ConclusionsIntervention by ANIT can significantly change the homeostasis of BAs and FFAs. HQD and astragalosides exerted a hepatoprotective effect against cholestatic liver injury by restoring the altered BA and FFA metabolism through the improvement of BA transporter, nucleus hormone receptor, and membrane receptor.

Interindividual Differences in Human Intestinal Microbial Conversion of (-)-Epicatechin to Bioactive Phenolic Compounds.

To quantify interindividual differences in the human intestinal microbial metabolism of (−)-epicatechin (EC), in vitro anaerobic incubations with fecal inocula from 24 healthy donors were conducted. EC-derived colonic microbial metabolites were qualitatively and quantitively analyzed by liquid chromatography triple quadrupole mass spectrometry (LC-TQ-MS) and liquid chromatography time-of-flight mass spectrometry (LC-TOF-MS). Quantitative microbiota characterization was achieved by 16S rRNA analysis. The results obtained show 1-(3′,4′-dihydroxyphenyl)-3-(2″,4″,6″-dihydroxyphenyl)-2-propanol (3,4-diHPP-2-ol) and 5-(3′,4′-dihydroxyphenyl)-γ-valerolactone (3,4-diHPV) to be key intermediate microbial metabolites of EC and also revealed the substantial interindividual differences in both the rate of EC conversion and the time-dependent EC metabolite pattern. Furthermore, substantial differences in microbiota composition among different individuals were detected. Correlations between specific microbial phylotypes and formation of certain metabolites were established. It is concluded that interindividual differences in the intestinal microbial metabolism of EC may contribute to interindividual differences in potential health effects of EC-abundant dietary foods or drinks.

Ferrous-activated persulfate oxidation of triclosan in soil and groundwater: The roles of natural mineral and organic matter

Contamination of antimicrobial agents such as Triclosan (TCS) in soil and groundwater possess high risk to human health and ecological systems. Present study systematically studied the degradation of TCS in soil and groundwater by Fe2+ activated persulfate (Fe2+/PS) oxidation process and special attention was paid on revealing the influence of remediation process on soil physicochemical and microbial characteristics. Experimental results demonstrated that TCS was readily degraded in soil upon Fe2+/PS oxidation system. Higher Fe2+/PS concentration and lower pH value may promote the TCS degradation. Besides added Fe2+, the naturally present Fe (III)-O and dissolved Fe from iron containing minerals may also activate PS for TCS degradation. SO4•−, HO•, R• and 1O2 were identified to be involved in the reaction system while addition of Fe2+-chelating agents, e.g., oxalic acid and ethylene diamine tetraacetic acid (EDTA) may slightly promote the degradation. Low concentration of Cl− facilitated TCS degradation and high concentration of Cl− slowed down the degradation. The presence of HCO3− may inhibit the degradation. Fe2+/PS oxidation process may partly reduce the soil organic matter content and diversely affect the composition of various C functional groups on soil. It also induced the breakdown of large soil aggregates and reduced the soil porosity, especially at macroporosity region. Phospholipid Fatty Acid test indicated that soil microbial community structure has been altered and the actinomycetes, fungi and Gram-negative bacteria decreased largely. The feasibility of remediation of TCS using Fe2+/PS oxidation in various natural groundwater samples was evaluated. Finally, five degradation intermediates of TCS by Fe2+/PS oxidation in soil were enriched by solid phase extraction and were identified by liquid chromatography-triple quadrupole mass spectrometry for proposing detailed transformation pathways.

Hypolipidemic effect of Alisma orientale (Sam.) Juzep on gut microecology and liver transcriptome in diabetic rats.

Alisma orientale (Sam.) Juzep (A. orientale) is a traditional herb that is often used to treat disease including edema and hyperlipidemia. However, the molecular mechanism by which Alisma orientale (Sam.) Juzep exerts its hypolipidemic effects remains unclear. In this study, a diabetic rat model was established by feeding a high-fat and high-sugar diet combined with a low-dose streptozotocin injection (HFS). Then the rats were treated with an A. orientale water extract (AOW), an A. orientale ethanolic extract (AOE) or metform (MET). The gut microflora and liver transcriptome were analyzed by high-throughput next-generation sequencing. Ultra-performance liquid chromatography-triple quadrupole-mass spectrometry was employed to analyze the major compounds in the AOE. The results showed that the serum total cholesterol (TC) and low density lipoprotein cholesterol (LDL-C) levels in rats of the AOE group (2.10 g/kg/day, 14 days) were significantly lower than those in the HFS group (p<0.01). Moreover, AOE treatment altered the gut microecology, particularly modulating the relative abundance of gut microflora involved in lipid metabolism compared with the HFS group. Furthermore, compared with the HFS group, the mRNA expression levels of Fam13a, Mapk7, Mpp7, Chac1, Insig1, Mcpt10, Noct, Greb1l, Fabp12 and Hba-a3 were upregulated after the administration of AOE. In contrast, the mRNA expression levels of Lox, Mybl1, Arrdc3, Cyp4a2, Krt20, Vxn, Ggt1, Nr1d1 and S100a9 were downregulated. Moreover, AOE treatment for two weeks markedly promoted the relative abundance of Lachnospiraceae (p = 0.0013). The triterpenoids contents in AOE were alisol A, alisol A 24-acetate, alisol B, alisol B 23-acetate, alisol C 23-acetate, alisol F, alisol F 24-acetate, and alisol G. Our findings above illustrated that the hypolipidemic effect of the triterpenoids of A. orientale is mediated mainly through alteration of the gut microecology and the regulation of genes involved in cholesterol metabolism, especially Insig1.

Matrix Reference Materials Development for Food Safety Application in Philippine Products

&lt;p&gt;The development of RMs was pioneered in the Philippines by the Industrial Technology Development Institute (ITDI) - DOST as part of its vision to establish metrological traceability and support the RMs needs of chemical testing laboratories in the country. Food safety issues for chemical testing of Philippine products were prioritized in this activity as these could affect the health of consumers and trade issues. Reference methods used for the provision of reference value was developed and validated for contaminants like histamine and benzoic acid in canned tuna and mango juice respectively. The materials were prepared and characterized and found to be homogeneous and stable for at least six (6) months. The reference value assigned to these RMs was done using a higher order method like isotope dilution technique coupled with Liquid Chromatography-Triple Quadrupole Mass Spectrometry (LCMSMS). Results were also cross-checked using gravimetric technique for High Performance Liquid Chromatography (HPLC) analysis. Certified RMs purchased from Metrology Institutes were also used to further support traceability of measurements. Philippine product RMs were developed for histamine and benzoic acid. The measurement traceability was disseminated by ITDI to local testing laboratories through the Proficiency Test schemes organized and conducted for the said analytes. &lt;/p&gt;

Tobacco smoke is a likely source of lead and cadmium in settled house dust

IntroductionEnvironmental exposure to lead (Pb) and cadmium (Cd) are risk factors for adverse health outcomes in children and adults. This study examined whether thirdhand smoke residue contributes to Pb and Cd in settled house dust. MethodsParticipants were 60 multiunit housing residents in San Diego, California. All had indoor smoking bans during the study period, and 55 were nonsmokers. Wipe samples from different surfaces and vacuum floor dust samples were analyzed for nicotine, a marker of thirdhand smoke, and for Pb and Cd using liquid chromatography-triple quadrupole mass spectrometry and inductively coupled plasma-mass spectrometry, respectively. ResultsExamined in each sample type separately, Pb and Cd loadings were significantly correlated (r = 0.73, vacuum floor dust; 0.52, floor wipes; 0.72, window sill/trough wipes; all p < 0.0025). Pb and Cd loadings from different sample types were not correlated (all p > 0.30). Nicotine loading in dust was significantly correlated with Pb and Cd loading in dust (r = 0.49 for Pb; r = 0.39 for Cd, all p < 0.0025). Pb and Cd loadings on floor or window surfaces, showed no association with nicotine loading in dust, on floors, or on furniture (all p < 0.30). ConclusionsTobacco smoke is a likely source of Pb and Cd that accumulates in settled house dust in multiunit housing, suggesting that Pb and Cd are constituents of thirdhand smoke that lingers long after smoking has ended.