Adaptive Neural Control for Hysteretic Nonlinear Systems With Hysteresis Neural Direct Inverse Compensator and Its Application.

Aiming at high precision control for a class of hysteretic nonlinear systems, a new hysteresis direct inverse compensator-based adaptive output feedback control scheme is designed in this article. First, a novel long short-term memory neural network (LSTMNN)-based hysteresis inverse compensator is established to compensate the asymmetric hysteresis nonlinearity, where the LSTMNN is used as the prediction mechanism for model operator weights, rather than the overall mapping of hysteresis input and output. Second, by designing the modified high-gain K -Filter states observer and the error transformed function, the unmeasurable states are estimated with arbitrarily small estimation error and the prespecified tracking performance is achieved. Lastly, the biconical dielectric elastomer actuator (DEA) motion platform is constructed. Then, the effectiveness of the proposed LSTMNN-based hysteresis inverse compensator and control scheme are verified on the experimental platform. The experimental results illustrate the effectiveness and advantages of proposed control scheme.

Hunting Metabolic Biomarkers for Exposure to Per- and Polyfluoroalkyl Substances: A Review.

Per- and polyfluoroalkyl substances (PFAS) represent a class of persistent synthetic chemicals extensively utilized across industrial and consumer sectors, raising substantial environmental and human health concerns. Epidemiological investigations have robustly linked PFAS exposure to a spectrum of adverse health outcomes. Altered metabolites stand as promising biomarkers, offering insights into the identification of specific environmental pollutants and their deleterious impacts on human health. However, elucidating metabolic alterations attributable to PFAS exposure and their ensuing health effects has remained challenging. In light of this, this review aims to elucidate potential biomarkers of PFAS exposure by presenting a comprehensive overview of recent metabolomics-based studies exploring PFAS toxicity. Details of PFAS types, sources, and human exposure patterns are provided. Furthermore, insights into PFAS-induced liver toxicity, reproductive and developmental toxicity, cardiovascular toxicity, glucose homeostasis disruption, kidney toxicity, and carcinogenesis are synthesized. Additionally, a thorough examination of studies utilizing metabolomics to delineate PFAS exposure and toxicity biomarkers across blood, liver, and urine specimens is presented. This review endeavors to advance our understanding of PFAS biomarkers regarding exposure and associated toxicological effects.

Effect of oral glucose tolerance test-based insulin resistance on embryo quality in women with/without polycystic ovary syndrome.

Objective: To explore the effects of insulin resistance (IR) on embryo quality and pregnancy outcomes in women with or without polycystic ovary syndrome (PCOS) undergoing in vitro fertilization (IVF)/intracytoplasmic sperm injection (ICSI). Methods: A retrospective cohort study concerning patients with/without PCOS who received gonadotropin-releasing hormone (GnRH)-antagonist protocol for IVF/ICSI from January 2019 to July 2022 was conducted. All the patients included underwent oral glucose tolerance test plus the assessment of insulin release within 6 months before the controlled ovarian stimulation. The Matsuda Index was calculated to diagnose IR. Two populations (PCOS and non-PCOS) were included and each was divided into IR and non-IR groups and analyzed respectively. The primary outcome was the high-quality day 3 embryo rate. Results: A total of 895 patients were included (751 with PCOS and 144 without PCOS). For patients with PCOS, the IR group had a lower high-quality day 3 embryo rate (36.8% vs. 39.7%, p=0.005) and available day 3 embryo rate (67.2% vs. 70.6%, p<0.001). For patients without PCOS, there was no significant difference between the IR and non-IR groups in high-quality day 3 embryo rate (p=0.414) and available day 3 embryo rate (p=0.560). There was no significant difference in blastocyst outcomes and pregnancy outcomes for both populations. Conclusion: Based on the diagnosis by the Matsuda Index, IR may adversely affect the day 3 embryo quality in patients with PCOS but not pregnancy outcomes. In women without PCOS, IR alone seems to have less significant adverse effects on embryo quality than in patients with PCOS. Better-designed studies are still needed to compare the differences statistically between PCOS and non-PCOS populations.

Investigations of the highly efficient processing technique, chemical constituents, and anti-inflammatory effect of N-ethyl-2-pyrrolidinone-substituted flavan-3-ol (EPSF)-enriched white tea.

N-Ethyl-2-pyrrolidinone-substituted flavan-3-ols (EPSFs) are a newly discovered compound class in tea with various bioactivities. This study aimed to develop a novel processing technique to enhance EPSF contents in white tea efficiently. Using optimal processing parameters of 125 °C and 30 min in a high-temperature sterilizing oven, total EPSF content significantly increased by 1.42-18.80-fold to 1.57-6.22 mg/g without impacting sensory characteristics. Metabolomics analysis revealed elevated levels of nucleosides, nucleotides, bases, theaflavins, flavonol aglycones, EPSFs, and most flavone-C-glycosides, as well as decreased levels of amino acids, procyanidins, theasinensins, several flavanols, and flavonol-O-glycosides after EPSF-enrichment treatment. Furthermore, the EPSF-enriched white tea exhibited notable anti-inflammatory effects, mitigating xylene-induced ear edema in mice and carrageenan-induced paw edema and cotton ball-induced granulomas in rats. This study developed a new processing technique for highly efficient enhancement of EPSFs in white tea and demonstrated that EPSF-enriched white tea has a potential to serve as effective anti-inflammatory dietary supplement.

Sesamin ameliorates nonalcoholic hepatic steatosis by inhibiting CD36-mediated hepatocyte lipid accumulation in vitro and in vivo.

Hepatic steatosis is a critical factor in the development of nonalcoholic steatohepatitis (NASH). Sesamin (Ses), a functional lignan isolated from Sesamum indicum, possesses hypolipidemic, liver-protective, anti-hypertensive, and anti-tumor properties. Ses has been found to improve hepatic steatosis, but the exact mechanisms through which Ses achieves this are not well understood. In this study, we observed the anti-hepatic steatosis effects of Ses in palmitate/oleate (PA/OA)-incubated primary mouse hepatocytes, AML12 hepatocytes, and HepG2 cells, as well as in high-fat, high-cholesterol diet-induced NASH mice. RNA sequencing analysis revealed that cluster of differentiation 36 (CD36), a free fatty acid (FA) transport protein, was involved in the Ses-mediated inhibition of hepatic fat accumulation. Moreover, the overexpression of CD36 significantly increased hepatic steatosis in both Ses-treated PA/OA-incubated HepG2 cells and NASH mice. Furthermore, Ses treatment suppressed insulin-induced de novo lipogenesis in HepG2 cells, which was reversed by CD36 overexpression. Mechanistically, we found that Ses ameliorated NASH by inhibiting CD36-mediated FA uptake and upregulation of lipogenic genes, including FA synthase, stearoyl-CoA desaturase 1, and sterol regulatory element-binding protein 1. The findings of our study provide novel insights into the potential therapeutic applications of Ses in the treatment of NASH.

Effects of different gonadotropin preparations in GnRH antagonist protocol for patients with polycystic ovary syndrome during IVF/ICSI: a retrospective cohort study.

Purpose: To compare the effects of recombinant FSH alfa (rFSH-alfa), rFSH-beta, highly purified human menopausal gonadotropin (HP-hMG) and urinary FSH (uFSH) in women with polycystic ovarian syndrome who have undertaken the GnRH antagonist protocol during IVF/ICSI treatment. Method: A single-center retrospective cohort study including women with PCOS who received the GnRH antagonist protocol from January 2019 to July 2022 was conducted. Patients were divided into rFSH-alfa group, HP-hMG group, uFSH group, and rFSH-beta group, and the number of oocytes retrieved, clinical pregnancy rate of the fresh cycle (primary outcomes), embryo quality, and severe OHSS rate (secondary outcomes) were compared. Results: No statistical differences were found among the four groups in fresh cycle clinical pregnancy rate (p=0.426), nor in the subgroup analyses. The HP-hMG group had a smaller number of oocytes retrieved and a higher high-quality D3 embryo rate than the three FSH groups (p<0.05). No statistical differences were found among the four groups in the severe OHSS rate (p=0.083). Conclusion: For women with PCOS undergoing the GnRH antagonist protocol, the clinical pregnancy rates of fresh IVF/ICSI-ET cycle are similar for all four types of Gn. With a lower risk of OHSS and a similar number of high-quality and available embryos, HP-hMG may have an advantage in the PCOS population.

[Optimization and application of determination method of cholesterol in various dishes].

OBJECTIVE: To establish a rapid and accurate method for the determination of cholesterol in a variety of finished dishes. METHODS: The samples were saponified with ethanol and potassium hydroxide solution at 80 ℃ for 0.5 h, then vortexed and mixed fully with ultrapure water, and extracted twice with 25 mL n-hexane. The extracting solution were evaporated to dryness under vacuum and redissolved by ethanol, finally determined by gas chromatograph. The sample loading solution was separated by HP-5 capillary column(30 m×0.25 mm, 0.25 µm) and quantified with external standard method. RESULTS: The method had good linearity in the concentration range of 2.5-250 µg/mL for cholesterol and the correlation coefficient was 0.9999. The detection limit was 0.25 mg/100 g edible part, and the limit of quantification was 0.75 mg/100 g edible part. Three representative samples were picked for spiked recovery experiments with three concentration levels according to their content of cholesterol. The average recovery rates ranged from 91.1% to 101%, and the relative standard deviations were not more than 5%. The content range of cholesterol in 15 vegan dishes was from negative to 10.3 mg/100 g edible part, in 14 dishes contained meat and vegetable was from 2.34 to 80.2 mg/100 g edible part and in 9 pure meat dishes was from 25.4 to 288 mg/100 g edible part. CONCLUSION: Compared with the national standard method, the method is simple to operate and more friendly to the experimenter while ensuring the accuracy and sensitivity requirements. It can meet the needs of efficient batch determination of cholesterol in a variety of finished dishes.

Simultaneous Determination of 12 Preservatives in Pastries Using Gas Chromatography-Mass Spectrometry.

(1) Background: Preservatives may pose a potential threat to human health. To ensure food safety, this study has devised a method that concurrently detects a dozen preservatives (acetic acid, propionic acid, dehydroacetic acid, benzoic acid, sorbic acid, dimethyl fumarate, methyl parahydroxybenzoate, ethyl parahydroxybenzoate, propyl parahydroxybenzoate, isopropyl parahydroxybenzoate, butyl parahydroxybenzoate, and isobutyl parahydroxybenzoate) in pastry, utilizing gas chromatography-mass spectrometry. (2) Methods: The pastry samples were acidified with hydrochloric acid, extracted with acetonitrile via vortexing, purified by hexane and saturated with sodium chloride solution to remove lipids and impurities, and then concentrated via nitrogen blowing. The method was then quantitatively analyzed using GC-MS with the internal standard method after methanol re-dissolution. (3) Results: The results showed that the content of the 12 preservatives had good linearity within the range of 1.0-50 µg/mL, with correlation coefficients all greater than 0.99. The method detection limit was 0.04-2.00 mg/kg and the quantification limit was 0.12-6.67 mg/kg. The average recovery rates of the samples at three different spiked concentrations of low, medium, and high were 70.18-109.22%, and the relative standard deviations were 1.82-9.79% (n = 6). (4) Conclusions: This method requires a small amount of sample, has high sensitivity, and is simple and fast to operate, making it suitable for the simultaneous determination of 12 preservatives in pastry. This approach contributes to the effective surveillance and regulation of preservative usage in pastries, thereby safeguarding public well-being.

Optimization of Physical Refining Process of Camellia Oil for Reduction of 3-Monochloropropane-1,2-Diol (3-MCPD) Ester Formation Using Response Surface Methodology on a Laboratory Scale.

Refined and deodorized camellia oil has been reported to contain a high amount of 3-monochloropropane-1,2-diol esters (3-MCPDE) due to the high-temperature deodorization step. To reduce 3-MCPDE in camellia oil, the physical refining process of camellia oil was simulated on a laboratory scale. Response surface methodology (RSM) was designed to modify and optimize the refining process with five processing parameters (water degumming dosage, degumming temperature, activated clay dosage, deodorization temperature and deodorization time). The optimized new refining approach achieved a 76.9% reduction in 3-MCPDE contents, in which the degumming moisture was 2.97%, the degumming temperature was 50.5 °C, the activated clay dosage was 2.69%, the deodorizing temperature was 230 °C, and the deodorizing time was 90 min. A significance test and analysis of variance results demonstrated that the deodorization temperature and deodorization time contributed significantly to the reduction of 3-MCPD ester. The joint interaction effects of activated clay dosage and deodorization temperature were significant for 3-MCPD ester formation.

Determination of ß2-Agonist Residues in Fermented Ham Using UHPLC-MS/MS after Enzymatic Digestion and Sulfonic Resin Solid Phase Purification.

ß2-agonists are a class of synthetic sympathomimetic drugs with acute poisoning effects if consumed as residues in foods. To improve the efficiency of sample preparation and to overcome matrix-dependent signal suppression in the quantitative analysis of four ß2-agonists (clenbuterol, ractopamine, salbutamol, and terbutaline) residues in fermented ham, an enzyme digestion coupled cation exchange purification method for sample preparation was established using ultra-high performance liquid chromatography and tandem mass spectrometry (UHPLC-MS/MS). Enzymatic digests were subject to cleanup treatment on three different solid phase extraction (SPE) columns and a polymer-based strong cation resin (SCR) cartridge containing sulfonic resin was found to be optimal compared with silica-based sulfonic acid and polymer sulfonic acid resins based SPEs. The analytes were investigated over the linear range of 0.5 to 10.0 µg/kg with recovery rates of 76.0-102.0%, and a relative standard deviation of 1.8-13.3% (n = 6). The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 µg/kg and 0.3 µg/kg, respectively. This newly developed method was applied to the detection of ß2-agonist residues in 50 commercial ham products and only one sample was found to contain ß2-agonist residues (clenbuterol at 15.2 µg/kg).

Effect of Hydroxychloroquine on Lupus Activity, Preeclampsia and Intrauterine Growth Restriction in Pregnant Women with Systemic Lupus Erythematosus and/or Antiphospholipid Syndrome: A Systematic Review and Meta-Analysis.

BACKGROUND: Hydroxychloroquine (HCQ) has been used in the treatment of systematic lupus erythematosus (SLE) and antiphospholipid syndrome (APS), but its effect on lupus activity during pregnancy, preeclampsia and intrauterine growth restriction (IUGR) remains unclear. METHODS: PubMed, Embase and Cochrane databases were searched before 11 September 2022 for randomized clinical trials (RCT) or observational studies involving additional HCQ treatment and pregnant women diagnosed as having SLE and/or APS/positive antiphospholipid antibodies (aPLs). Risks of high lupus activity, preeclampsia and IUGR were explored. RESULTS: One RCT and 13 cohort studies were included. A total of 1764 pregnancies were included in the pooled meta-analysis (709 in the HCQ group vs. 1055 in the control group). After the additional use of HCQ, the risk of high lupus activity decreased (RR: 0.74, 95% CI: 0.57-0.97, p = 0.03). For preeclampsia, the total incidence decreased (RR: 0.54, 95% CI: 0.37-0.78, p = 0.001). The subgroup analysis showed statistical significance in the SLE subgroup (RR: 0.51, 95% CI: 0.34-0.78, p = 0.002) but not in the APS/aPLs subgroup (RR: 0.66, 95% CI: 0.29-1.54, p = 0.34). For IUGR, the decrease in incidence was not statistically significant (RR: 0.80, 95% CI: 0.47-1.35, p = 0.46), neither in the SLE subgroup (RR: 0.74, 95% CI: 0.40-1.36, p = 0.33) nor in the APS/aPLs subgroup (RR: 1.26, 95% CI: 0.34-4.61, p = 0.73). CONCLUSION: The additional use of HCQ may decrease the risk of high lupus activity during pregnancy and the incidence of preeclampsia for SLE patients, but the results do not support that using HCQ decreases the incidence of preeclampsia for APS/aPLs patients or reduces IUGR risk for SLE and/or APS/aPLs patients.

Acute Developmental Toxicity of Panax notoginseng in Zebrafish Larvae.

OBJECTIVE: To evaluate toxicity of raw extract of Panax notoginseng (rPN) and decocted extract of PN (dPN) by a toxicological assay using zebrafish larvae, and explore the mechanism by RNA sequencing assay. METHODS: Zebrafish larvae was used to evaluate acute toxicity of PN in two forms: rPN and dPN. Three doses (0.5, 1.5, and 5.0 µ g/mL) of dPN were used to treat zebrafishes for evaluating the developmental toxicity. Behavior abnormalities, body weight, body length and number of vertebral roots were used as specific phenotypic endpoints. RNA sequencing (RNA-seq) assay was applied to clarify the mechanism of acute toxicity, followed by real time PCR (qPCR) for verification. High performance liquid chromatography analysis was performed to determine the chemoprofile of this herb. RESULTS: The acute toxicity result showed that rPN exerted higher acute toxicity than dPN in inducing death of larval zebrafishes (P<0.01). After daily oral intake for 21 days, dPN at doses of 0.5, 1.5 and 5.0 µ g/mL decreased the body weight, body length, and vertebral number of larval zebrafishes, indicating developmental toxicity of dPN. No other adverse outcome was observed during the experimental period. RNA-seq data revealed 38 genes differentially expressed in dPN-treated zebrafishes, of which carboxypeptidase A1 (cpa1) and opioid growth factor receptor-like 2 (ogfrl2) were identified as functional genes in regulating body development of zebrafishes. qPCR data showed that dPN significantly down-regulated the mRNA expressions of cpa1 and ogfrl2 (both P<0.01), verifying cpa1 and ogfrl2 as target genes for dPN. CONCLUSION: This report uncovers the developmental toxicity of dPN, suggesting potential risk of its clinical application in children.

Optimization of pretreatment methods for N-nitrosamine compounds in ready-to-eat aquatic products / 预防医学

Objective@#To optimize the pretreatment method of N-nitrosamine compounds in ready-to-eat aquatic products. @*Methods@#Market-sold ready-to-eat aquatic products were collected, homogenized and distilled by steam. The samples were extracted for 10 minutes using dispersive liquid-liquid microextraction (DLLME) with ethanol, trichloromethane and sodium chloride (3.0 g). After centrifugation, the organic phase in the lower layer was collected and subjected to gas chromatography-tandem mass spectrometry (GC-MS/MS). The six common N-nitrosamine compounds were determined in ready-to-eat aquatic products using multiple reaction monitoring mode (MRM) and quantified by the internal standard method. @*Results@#The optimized method exhibited a good linear relationship at concentrations of 10.0 to 500 μg/L for determination of 6 N-nitrosamine compounds (correlation coefficient of greater than 0.999), with 0.05 to 0.60 μg/kg limit of detection, 0.15 to 1.60 μg/kg limit of quantitation, mean spiked recovery rates of 71.8% to 108.9%, and relative standard deviations of 1.4% to 8.6%. N-Nitrosodimethylamine showed the highest detection rate in 20 market-sold ready-to-eat aquatic products (90%), and the detection rates of N-Nitrosopyrrolidine, N-Nitrosodiethylamine and N-dibutylnitrosamine were 15%, 10% and 10%, respectively. @*Conclusion@#Steam distillation combined with DLLME may optimize the pretreatment method of N-nitrosamine compounds in ready-to-eat aquatic products and meet the measurement requirements.

Adaptive responses drive the success of polyploid yellowcresses (Rorippa, Brassicaceae) in the Hengduan Mountains, a temperate biodiversity hotspot.

Polyploids contribute substantially to plant evolution and biodiversity; however, the mechanisms by which they succeed are still unclear. According to the polyploid adaptation hypothesis, successful polyploids spread by repeated adaptive responses to new environments. Here, we tested this hypothesis using two tetraploid yellowcresses (Rorippa), the endemic Rorippa elata and the widespread Rorippa palustris, in the temperate biodiversity hotspot of the Hengduan Mountains. Speciation modes were resolved by phylogenetic modeling using 12 low-copy nuclear loci. Phylogeographical patterns were then examined using haplotypes phased from four plastid and ITS markers, coupled with historical niche reconstruction by ecological niche modeling. We inferred the time of hybrid origins for both species as the mid-Pleistocene, with shared glacial refugia within the southern Hengduan Mountains. Phylogeographic and ecological niche reconstruction indicated recurrent northward colonization by both species after speciation, possibly tracking denuded habitats created by glacial retreat during interglacial periods. Common garden experiment involving perennial R. elata conducted over two years revealed significant changes in fitness-related traits across source latitudes or altitudes, including latitudinal increases in survival rate and compactness of plant architecture, suggesting gradual adaptation during range expansion. These findings support the polyploid adaptation hypothesis and suggest that the spread of polyploids was aided by adaptive responses to environmental changes during the Pleistocene. Our results thus provide insight into the evolutionary success of polyploids in high-altitude environments.

A novel single step solid-phase extraction combined with bromine derivatization method for rapid determination of acrylamide in coffee and its products by stable isotope dilution ultra-performance liquid chromatography tandem triple quadrupole electrospray ionization mass spectrometry.

This work aimed to establish a novel determination method for acrylamide in coffee and its products by ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). Acrylamide in samples were prepared by a single-step solid-phase extraction clean-up using mixed mode sorbents. The bromine derivatization efficiency of acrylamide and its internal standard were improved at an acidic condition. After derivation, the retention capability of acrylamide and its resistance to interference were significantly improved. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.2 and 4 µg/kg for roasted and instant coffees, while they were 0.24 and 0.8 µg/kg for ready-to-drink coffees. The average recoveries for acrylamide ranged from 99.3 to 102.2% in coffee and its products. All the results showed that the developed method was simple, quick, specific and suitable for screening and determination of acrylamide in batch samples of coffee and its products.

Determination of Polycyclic Aromatic Hydrocarbons in Traditional Chinese Medicine Raw Material, Extracts, and Health Food Products.

The four polycyclic aromatic hydrocarbon markers (PAH4) of benzo[a]anthracene (BaA), chrysene (Chr), benzo[b]fluoranthene (BbF), and benzo[a]pyrene (BaP) are indicators showing polycyclic aromatic hydrocarbon (PAH) contamination levels in Chinese medicine raw materials (CMRMs), extracts and health food products; Samples of herbal medicine, herbal extracts, and food supplements were extracted with n-hexane, then cleaned up sequentially on Florisil and EUPAH solid-phase extraction (SPE) columns. A gas chromatography-mass spectrometry method for the determination of four polycyclic aromatic hydrocarbon markers in Chinese medicine raw material, extracts, and health food products was established; In spiked-recovery experiments, the average recovery was about 78.6-107.6% with a precision of 2.3-10.5%. The limit of quantification (LOQ) and limit of detection (LOD) of the PAH4 markers in this method were 2.0 µg/kg and 0.7 µg/kg, respectively. When the developed method was utilized to determine PAH4 contents in 12 locally available health food products, 3 samples contained over 10.0 µg/kg BaP, and 5 samples contained over 50.0 µg/kg PAH4. The European Union (EU) limits for BaP and PAH4 are 10 and 50.0 µg/kg, respectively; therefore, more attention must be drawn to the exposure risk of BaP and PAH4 in CMRMs, their extracts, and health food products. According to the risk assessment based on the Margin of Exposure (MOE) method, it is recognized that the products mentioned in this study pose a low risk.

Determination of 15 + 1 European Priority Polycyclic Aromatic Hydrocarbons in Smoked Meat Products by Saponification/Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry.

A method for the determination of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in smoked meat samples by saponification/solid-phase extraction and gas chromatography-mass spectrometry has been developed. Both saponification and solid-phase extraction conditions were optimized, which lead to shorter sample preparation time and excellent sensitivity and selectivity. The optimal saponification condition for the lipid extract of 5.00 g smoked food sample was 5 mL KOH (1.5 mol/L)-ethanol at 70°C for 5 min, and the shorter alkaline treatment time avoided the loss of volatile EUPAHs such as Benzo[c]fluorene. All the EUPAHs showed good linearity in the range between 5.0 and 50.0 ng/mL with correlation coefficients between 0.997 and 1.00. The estimated LODs for the EUPAHs were 0.15-0.30 µg/kg, while the LOQs were 0.50-1.0 µg/kg. The three spiking levels of EUPAHs were 1.0, 2.0 and 5.0 µg/kg, and the average recovery was between 75.2 and 99.6%, while the RSD were 2.3-12.4%. This sensitive and rapid method was successfully applied to smoked meat samples from Zhejiang Province of China, and the results revealed the presence of 13 EUPAHs. Benzo[a]pyrene (BaP) was found in 19 out of 20 samples, with concentration ranging from 0.51 to 4.57 µg/kg. The sum of concentrations of PAH4 (summation of benzo(a)pyrene, chrysene, benzo(a)anthracene, and benzo(b)fluoranthene) were 2.40-53.56 µg/kg.

[Characterization and investigation of 16 European priority polycyclic aromatic hydrocarbons in commercial infant formula milk powder in Hangzhou].

OBJECTIVE: A gas chromatography-mass spectrometry(GC-MS) method for the determination of 16 European priority polycyclic aromatic hydrocarbons(16 EUPAHs) in infant formula milk powder was established, and the characterization and investigation of 16 EUPAHs in 70 milk formula powders were carried out in 2020. METHODS: After hydrolysis, extraction, saponification and solid phase extraction, infant formula milk powder was detected by GC-MS using DB-EUPAH capillary column(20 m×0.18 mm, 0.14 µm)and quantified by internal standard method. RESULTS: The average recoveries ranged from 67.8% to 116.2% and the relative standard deviations ranged from 2.0% to 15.1%(n=6). The limits of quantification and detection of the method were 0.5 and 0.2 µg/kg, respectively. The content of 16 EUPAHs was <0.2-0.48 µg/kg, including PAH4 content in the range of <0.2-0.91 µg/kg, the characterization and investigation of infant formula powder in 16 EUPAHs mainly chrysene, cyclopenta[c, d]pyrene, benz[a]anthracene, benzo[b]fluoranthene, benzo[g, h, i]perylene. CONCLUSION: The method is simple, accurate and suitable for the determination of 16 EUPAHs in infant formula milk powder. The result showed that the content of 16 EUPAHs in commercially available infant formula milk powder in Hangzhou was low and all of them met the limit requirement of European Union.

Metabolomics Analysis Reveals Four Novel N-Ethyl-2-pyrrolidinone-Substituted Theaflavins as Storage-Related Marker Compounds in Black Tea.

Tea market is currently oversupplied, and unsold tea often needs to be properly stored for a period of time. However, the chemical changes occurring in black tea during storage are limitedly understood. In this study, a comprehensive nontargeted and targeted metabolomics approach was used to investigate the dynamic changes in compounds in time-series (0-19 months)-stored black teas. The contents of flavanols, theaflavins (TFs), theasinensins, procyanidins, most phenolic acids, amino acids, quercetin-O-glycosides, and myricetin-O-glycosides decreased during storage, while the contents of N-ethyl-2-pyrrolidinone-substituted flavanols, flavone-C-glycosides, and most kaempferol-O-glycosides increased. More importantly, four novel compounds strongly positively correlated with storage duration (r = 0.922-0.969) were structurally assigned as N-ethyl-2-pyrrolidinone-substituted TFs and validated with synthetic reactions of TFs and theanine standards. The content of N-ethyl-2-pyrrolidinone-substituted TFs was 51.54 µg/g in black tea stored for 19 months. To the best of our knowledge, N-ethyl-2-pyrrolidinone-substituted TFs were discovered in tea for the first time.