Osteocyte ferroptosis induced by ATF3/TFR1 contributes to cortical bone loss during ageing.

Cortical bone loss is intricately associated with ageing and coincides with iron accumulation. The precise role of ferroptosis, characterized by iron overload and lipid peroxidation, in senescent osteocytes remains elusive. We found that ferroptosis was a crucial mode of osteocyte death in cortical bone during ageing. Using a single-cell transcriptome analysis, we identified activating transcription factor 3 (ATF3) as a critical driver of osteocyte ferroptosis. Elevated ATF3 expression in senescent osteocytes promotes iron uptake by upregulating transferrin receptor 1 while simultaneously inhibiting solute carrier family 7-member 11-mediated cystine import. This process leads to an iron overload and lipid peroxidation, culminating in ferroptosis. Importantly, ATF3 inhibition in aged mice effectively alleviated ferroptosis in the cortical bone and mitigated cortical bone mass loss. Taken together, our findings establish a pivotal role of ferroptosis in cortical bone loss in older adults, providing promising prevention and treatment strategies for osteoporosis and fractures.

Leaching characteristics and pollution risk assessment of potentially harmful elements from coal gangue exposed to weathering for different periods of time.

To explore the leaching behavior and potential degree of pollution that can result from the backfilling of goafs with different types of coal gangue (CG), fresh CG from the Hongqi Coal Mine goaf and surface CG (weathered for 1 year) were selected as the research objects in this study. A series of leaching experiments were carried out using the Ordovician limestone karst waters of the mining areas as the soaking solution. A comparative study on the dissolution characteristics of Fe3+, Mn2+, and SO42- and on the traditional water quality parameters of the two types of CG was conducted. The results showed that the soaked, weathered CG displayed a higher ion dissolution value than fresh CG. The ratio of each ion was as follows: Fe3+ was 1, Mn2+ was 2.86 ~ 68.18, and SO42- was 1.34 ~ 2.09. Over time, the ion concentration of water samples that initially contained high ion concentration values showed a decreasing trend after CG was soaked in these waters, but the values were still in the range of high ion release concentrations. The pH and oxidation‒reduction potential (ORP) values of the leachate of both CG types indicated that the leachates were weakly alkaline and weakly oxidizing, and the overall change in total dissolved solids (TDS) was small and consistent with the SO42- trend. SO42- in the leachate of the weathered CG showed a more significant correlation with the pH and TDS of the soaking solution, and it was the major pollutant. According to the geoaccumulation index evaluation, weathered CG had higher pollution potential than fresh CG. Fe3+ presented a slight and moderate risk for contamination.

Construction of Ultrafine Ag2S NPs Anchored onto 3D Network Rodlike Bi2SiO5 and Insight into the Photocatalytic Mechanism.

A novel three-dimensional (3D) network rodlike Ag2S/Bi2SiO5 photocatalyst with a p-n heterostructure composed of ultrafine Ag2S nanoparticles (NPs) and Bi2SiO5 nanosheets was prepared using an anionic self-regulation strategy by a two-step hydrothermal process. The architecture facilitated the efficient transfer and separation of photogenerated electron-hole pairs. The optimal Ag2S/Bi2SiO5 composite (ABSO0.10) exhibited an excellent reduction activity (93.5% Cr(VI) removal in wastewater containing 50 mg·L-1 Cr(VI) within 90 min under visible light), which was about 11.2 and 25.6 times higher than that of the pristine Ag2S and virgin Bi2SiO5, respectively. Assisted by experiments and density functional theory (DFT) calculations, a possible photocatalytic mechanism for Cr(VI) reduction over the Ag2S/Bi2SiO5 composite under visible-light irradiation was proposed.

Recyclable europium functionalized metal-organic fluorescent probe for detection of tryptophan in biological fluids and food products.

An europium functionalized metal-organic fluorescent probe, Eu3+@UiO-66-FDC was constructed by post-synthetic modification through coordination interactions. Eu3+@UiO-66-FDC displayed high selectivity and sensitivity toward Tryptophan (Trp) among all the 20 natural amino acids and other general compounds in food and biological samples, with a wide linear concentration range (0-1000 µM), low detection limit (0.29 µM), and a rapid response (<1 min). Besides, this probe was utilized to detect Trp in rabbit blood serum and milk samples with good recoveries, which were verified by high-performance liquid chromatography (HPLC). Notably, this fluorescent probe proved to be a recyclable material. Hence, this work provides a reliable and recyclable fluorescent probe applicable toward the detection of Trp in biological fluids and/or food products.

Transcriptome analysis of Phelipanche aegyptiaca seed germination mechanisms stimulated by fluridone, TIS108, and GR24.

P. aegyptiaca is one of the most destructive root parasitic plants worldwide, causing serious damage to many crop species. Under natural conditions P. aegyptiaca seeds must be conditioned and then stimulated by host root exudates before germinating. However, preliminary experiments indicated that TIS108 (a triazole-type inhibitor of strigolactone) and fluridone (FL, an inhibitor of carotenoid-biosynthesis) both stimulated the germination of P. aegyptiaca seeds without a water preconditioning step (i.e. unconditioned seeds). The objective of this study was to use deep RNA sequencing to learn more about the mechanisms by which TIS108 and FL stimulate the germination of unconditioned P. aegyptiaca seeds. Deep RNA sequencing was performed to compare the mechanisms of germination in the following treatments: (i) unconditioned P. aegyptiaca seeds with no other treatment, (ii) unconditioned seeds treated with 100 mg/L TIS108, (iii) unconditioned seeds treated with 100 mg/L FL + 100 mg/L GA3, (iv) conditioned seeds treated with sterile water, and (v) conditioned seeds treated with 0.03 mg/L GR24. The de novo assembled transcriptome was used to analyze transcriptional dynamics during seed germination. The key gene categories involved in germination were also identified. The results showed that only 119 differentially expressed genes were identified in the conditioned treatment vs TIS108 treatment. This indicated that the vast majority of conditions for germination were met during the conditioning stage. Abscisic acid (ABA) and gibberellic acid (GA) played important roles during P. aegyptiaca germination. The common pathway of TIS108, FL+GA3, and GR24 in stimulating P. aegyptiaca germination was the simultaneous reduction in ABA concentrations and increase GA concentrations. These results could potentially aid the identification of more compounds that are capable of stimulating P. aegyptiaca germination. Some potential target sites of TIS108 were also identified in our transcriptome data. The results of this experiment suggest that TIS108 and FL+GA3 could be used to control P. aegyptiaca through suicidal germination.

Simultaneous solid phase extraction coupled with liquid chromatography tandem mass spectrometry and gas chromatography tandem mass spectrometry for the highly sensitive determination of 15 endocrine disrupting chemicals in seafood.

This study aimed to develop a sensitive and reliable multi-residue method for the determination of trace amounts of endocrine disrupting chemicals including five phthalate esters (PAEs), five monoalky phthalate esters (MPEs), four alkylphenols (APs) and bisphenol A (BPA) in seafood. Ultrasonic liquid extraction was selected for extraction based on acetonitrile, instead of frequently-used n-hexane, due to its lower background of PAEs. Application of solid phase extraction (SPE) with primary secondary amine (PSA, 1g/6 mL) cartridge achieved the relatively low matrix effects for MPEs and BPA in seafood. To our knowledge, it is the first study reporting about simultaneous extraction and purification of PAEs, MPEs, APs and BPA in biota samples. To obtain the maximum sensitivity, both liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography tandem mass spectrometry (GC-MS/MS) were applied for analysis. This method was validated and tested on fish, mollusk and prawn. Sufficient linearity was verified by Mandel's fitting test for the matrix-matched calibrations used in this study for MPEs, APs and BPA, between 0.5 ng/g and 200 ng/g or 400 ng/g. And correlation coefficients of all calibrations suppressed 0.99 for all analytes. Good recoveries were obtained, ranging from 60% to 127% for most compounds. The sensitivity was good with method detection limits (MDLs) of 0.015-2.2 ng/g wet weight (ww) for all compounds. Most MDLs are much lower than those in previous reports. The sensitive method was then applied on real fish, mollusk and prawn samples from the Yangtze River Delta sea area (China), and all the target compounds were detected with the maximum concentrations of PAEs, MPEs, APs and BPA up to 219.3 ng/g ww, 51.4 ng/g ww, 62.0 ng/g ww and 8.6 ng/g ww, respectively.

Multi-class method for determination of veterinary drug residues and other contaminants in infant formula by ultra performance liquid chromatography-tandem mass spectrometry.

A rapid, simple and generic analytical method which was able to simultaneously determine 220 undesirable chemical residues in infant formula had been developed. The method comprised of extraction with acetonitrile, clean-up by low temperature and water precipitation, and analysis by ultra performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-ESI-MS-MS) using multiple reaction monitoring (MRM) mode. Most fat materials in acetonitrile extract were eliminated by low temperature clean-up. The water precipitation, providing a necessary and supplementary cleanup, could avoid losses of hydrophobic analytes (avermectins, ionophores). Average recoveries for spiked infant formula were in the range from 57% to 147% with associated RSD values between 1% and 28%. For over 80% of the analytes, the recoveries were between 70% and 120% with RSD values in the range of 1-15%. The limits of quantification (LOQs) were from 0.01 to 5 µg/kg, which were usually sufficient to verify the compliance of products with legal tolerances. Application of this method in routine monitoring programs would imply a drastic reduction of both effort and time.

Generic and rapid determination of veterinary drug residues and other contaminants in raw milk by ultra performance liquid chromatography-tandem mass spectrometry.

A generic, rapid and simple analytical method able to identify 255 veterinary drug residues and other contaminants in raw milk had been developed. The method was based on two-step simple precipitation and ultra performance liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (UPLC-ESI-MS/MS) operating both in positive and negative multiple reaction mode (MRM). For most of the target analytes, the optimized pretreatment processes led to no significant interference on analysis from complicated sample matrix. For quantification, matrix-fortified calibration curves were performed to compensate for the matrix effect and loss in sample preparation. Competent linearity was found for over 90% of target compounds with linear regression coefficients (R) higher than 0.99. Detection limits ranged from 0.05 to 10µg/kg. Average recoveries spiked into raw milk were in the range from 63% to 141% with associated RSD values from 1% to 29% under the selected conditions. The method had been validated for its extraction sensitivity, linearity, recoveries and precision. The results clearly demonstrated the feasibility of the approach proposed. Application of this method, which improved efficiency and coverage of residues, would imply a drastic reduction of both effort and time in routine monitoring programs.

MCX based solid phase extraction combined with liquid chromatography tandem mass spectrometry for the simultaneous determination of 31 endocrine-disrupting compounds in surface water of Shanghai.

A novel analytical method employing MCX (mixed-mode cationic exchange) based solid phase extraction (SPE) coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed to detect 31 endocrine-disrupting compounds (EDCs) in surface water samples simultaneously. The target EDCs belong to five classes, including seven estrogens, eight androgens, six progesterones, five adrenocortical hormones and five industrial compounds. In order to simultaneously concentrate the target EDCs and eliminate matrix interferences in the water samples, MCX SPE cartridges were employed for SPE, and then followed by a simple and highly efficient three-step sequential elution procedure. Two electrospray ionization (ESI) detection modes, positive (ESI+) and (ESI-), were optimized for HPLC-MS/MS analysis to obtain the highest sensitivity for all the EDCs. The limits of detection (LODs) were 0.02-1.9 ng L(-1), which are lower than or comparable to these reported in references. Wide linear ranges (LOD-100 ng L(-1) for ESI+ mode, and LOD-200 ng L(-1) for ESI- mode) were obtained with determination coefficients (R(2)) higher than 0.99 for all the compounds. With five internal standards, good recoveries (84.4-103.0%) of all the target compounds were obtained in selected surface water samples. The developed method was successfully applied to investigate the EDCs occurrence in the surface water of Shanghai by analyzing surface water samples from 11 sites. The results showed that nearly all the target compounds (30 in 31) were present in the surface water samples of Shanghai, of which three industrial compounds (4-t-OP, BPA, and BPF) showed the highest concentrations (median concentrations were 11.88-23.50 ng L(-1)), suggesting that industrial compounds were the dominating EDCs in the surface water of Shanghai, and much more attention should be paid on these compounds. Our present research demonstrated that SPE with MCX cartridges combined with HPLC-MS/MS was convenient, efficient and reliable for multiclass analysis of EDCs in surface water.

[Investigation on the molecular structures and electronic absorption spectra of Tanshinone II A and Tanshinone II A -Cu(II) complex].

Using an intensified spectroscopic detector CCD, the UV-Vis absorption spectra of tanshinone II A and Tanshinone II A-Cu(II) complex were acquired. The stable geometric structures of Tanshinone II A and Tanshinone II A -Cu(II) complex were obtained by using density functional theory method. Based on the optimized geometric structures, the electronic absorption spectra of Tanshinone II A and Tanshinone II A-Cu(II) complex in gas phase and in ethanol solution were calculated by using time-dependent density functional theory. Results show that the solvent effect induces the red shift of spectrum for Tanshinone II A and the blue shift of spectrum for Tanshinone II A-Cu(II) complex. The calculated absorption spectra including the solvent effect are in good agreement with the experimental results. The present work first measured and computed the electronic absorption spectra of Tanshinone II A-Cu(II) complex.

Dithizone-functionalized solid phase extraction-displacement elution-high performance liquid chromatography-inductively coupled plasma mass spectrometry for mercury speciation in water samples.

A novel and simple solid phase extraction (SPE)-high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) method was developed for determination of inorganic mercury (IHg), methylmercury MeHg and ethylmercury (EtHg) in water samples in the present work. The procedure involves pre-functionalization of the commercially available C18 SPE column with dithizone, loading water sample, displacement elution of mercury species by Na(2)S(2)O(3) solution, followed by HPLC-ICP-MS determination. Characterization and optimization of operation parameters of this new SPE procedure were discussed, including eluting reagent selection, concentration of eluting reagent, volume of eluting reagent, effect of NaCl and humic acid in sample matrix. At optimized conditions, the detection limits of mercury species for 100mL water sample were about 3ngL(-1) and the average recoveries were 93.7, 83.4, and 71.7% for MeHg, IHg and EtHg, respectively, by spiking 0.2microgL(-1) mercury species into de-ion water. Stability experiment reveals that both the dithizone-functionalized SPE cartridge and the mercury species incorporated were stable in the storage procedure. These results obtained demonstrate that SPE-HPLC-ICP-MS is a simple and sensitive technique for the determination of mercury species at trace level in water samples with high reproducibility and accuracy.

Effect of pulmonary autograft transplantation in the surgical treatment of aortic valve disease.

BACKGROUND: Aortic root replacement with pulmonary autograft (Ross procedure) has the advantages of good haemodynamics and growth potential without the need for anticoagulation. In this study, we reviewed our experience of the Ross procedure for patients with aortic valve disease. METHODS: From October 1994 to January 2005, 42 Ross procedures were performed in our centre. There were 30 males and 12 females. The mean age was 28 +/- 15 years (range, 5-56 years). Congenital heart disease (CHD) with aortic valve stenosis (AS) and/or aortic valve insufficiency (AI) in 40 cases including one associated with ventricular septal defect (VSD), degenerated aortic valve disease with AS in 1 and subacutive bacterial endocarditis (SBE) with AI in 1 were studied. The diagnosis was made by ultracardiography (UCG) in all patients. The mean aortic valve annulus diameter (AVD) was (2.45 +/- 0.31) cm and pulmonary valve annulus diameter (MPVD) was (2.34 +/- 0.21) cm. All patients had normal pulmonary valves. The New York Heart Association (NYHA) function class was II in 36 cases and III in 6 cases. The operation was performed under moderate hypothermic cardiopulmonary bypass (CPB) with aortic root replacement using pulmonary autograft and pulmonary valve replacement with a homograft. RESULTS: There was no early hospital mortality. Postoperative UCG showed normal aortic valve function in all our patients. The mean gradient across the aortic valve was (6.11 +/- 0.12) mmHg. The left ventricular diastole diameter (LVDD) decreased significantly from (62 +/- 5) mm to (56 +/- 3) mm (P < 0.001). The mean postoperative left ventricular ejective fraction (LVEF) was 0.49 +/- 0.23. All patients were in NYHA class I-II. Follow-up was completed in 38 cases for a mean period of 3.2 years (range 1-10 years). All survivors were in NYHA class I with normal neo-aortic and pulmonary valve function. One patient died after secondary operation due to homograft fungal endocarditis 1 year after the Ross procedure. The cause of death was uncontrolled bleeding. Another patient suffered from cardiogenic shock and was on extracorporeal membrane oxygenation (ECMO) for 10 days postoperatively. This patient was subsequently self-discharged from hospital due to financial issues and he was excluded from follow-up. CONCLUSION: The Ross procedure is an excellent technique to treat aortic valve disease. Our data show that it can be performed safely with good early and mid-term clinical outcomes.

Development of an automated on-line pre-column derivatization procedure for sensitive determination of histamine in food with high-performance liquid chromatography-fluorescence detection.

An improved sensitive method was developed and validated for the determination of histamine in food samples by using automated on-line pre-column derivatization coupled with high performance liquid chromatography and fluorescence detection (HPLC-FLD). o-Phthaldialdehyde (OPA) was adopted as derivatization reagent, and a "sandwich" (OPA+histamine+OPA) aspiration mode for the automated on-line pre-column derivatization was found to efficiently enhance the method sensitivity and precision. Histamine in food samples was efficiently extracted with a methanol-phosphate buffer solution (50:50, v/v) at 60 degrees C for 30 min, and purified with Waters Oasis MCX solid-phase extraction (SPE) cartridge. The limit of quantification for this method is 0.2 mg/kg, which is very sensitive for histamine determination. With the "sandwich" injection program, 3.7% of relative standard deviation (RSD) was achieved by five replicative determinations of a sample blank spiked with 0.25 mg/kg histamine standard. Histamine in food samples such as fumitory skipjack and mackerel was analyzed with relative recoveries over 95% at spiking level of 150 mg/kg, as well as canned tuna fish and cheese with relative recoveries up to 98% at spiking levels of 0.50 and 5.0 mg/kg, respectively. The proposed method was validated with a sample from the Food Analysis Performance Assessment Scheme (FAPAS) as a standard certified material; and the results (140+/-6 mg/kg) agreed well with the assigned value (139 mg/kg).

Direct determination of chlorophenols in environmental water samples by hollow fiber supported ionic liquid membrane extraction coupled with high-performance liquid chromatography.

The 1-octyl-3-methylimidazolium hexafluorophosphate ([C8MIM][PF6]) ionic liquid was immobilized in the pores of a polypropylene hollow fiber for hollow fiber-protected liquid-phase microextraction. Analytes including 4-chlorophenol (4-CP), 3-chorophenol (3-CP), 2,4-dichlorophenol (2,4-DCP) and 2,4,6-trichlorophenol (2,4,6-TCP) were extracted into this ionic liquid membrane, and back extracted into 10microL sodium hydroxide acceptor solution in the lumen of the hollow fiber. Then, the acceptor solution was withdrawn into the high-performance liquid chromatography (HPLC) microsyringe connected to the hollow fiber, and directly injected into the HPLC system for analysis. Some parameters that might affect the extraction efficiency were optimized, and low detection limits (0.5microgL(-1) for 4-CP, 3-CP, DCP and 1.0microgL(-1) for TCP) were obtained. Good repeatability was achieved because of the stability of the hollow fiber-supported ionic liquid membrane. The proposed procedure was applied for direct determination of the four chlorophenols in some real water samples including groundwater, river water, wastewater and tap water. All of the four chlorophenols in these water samples were under the limits of determination, and the recoveries were in the range of 70.0-95.7% at 5microgL(-1) spiked level.

Equilibrium sampling of freely dissolved alkylphenols into a thin film of 1-octanol supported on a hollow fiber membrane.

A new negligible depletion extraction procedure was proposed for equilibrium sampling of 4-tert-octylphenol (OP) and 4-nonylphenol (NP) into a thin film of 1-octanol supported on a hollow fiber membrane. This thin liquid film extraction technique was directed at the determination of (1) freely dissolved concentrations, (2) distribution coefficients to 1-octanol (D(ow)), and (3) binding to dissolved organic matter (DDOC). The sampling device was prepared by dipping pieces of polypropylene microporous hollow fiber membrane (10-mm length, 30-microm wall thickness, 240-microm inner diameter) into 1-octanol for a few seconds to impregnate the pores of the hollow fiber wall. After stirring in 100 mL of sample solution for 24 h, the sampling device was harvested and desorbed with 30 microL of methanol, of which 20 microL was injected for HPLC analysis. With the measured D(ow) of a chemical and its equilibrium concentration in the 1-octanol sampling phase (C(octanol)), the freely dissolved concentration (Cfree) was calibrated based on Cfree = C(octanol)/D(ow). Measured log Dow values of OP (4.32 +/- 0.06) and NP (4.79 +/- 0.02) were independent of the chemical concentration, only minimally affected by the environmentally relevant pH, buffering capacity, and salinity of samples, and agreed well with reported values. Log DDOC values of OP (4.89 +/- 0.43) and NP (5.14 +/- 0.37), determined in Aldrich humic acid solution, agreed with reported partition coefficients to organic carbon (log Koc) for particles in river water and effluent wastewater. Short equilibration times and high enrichment factors were obtained for both analytes due to the high surface to volume ratio of the new sampler. The technique was successfully applied to determine Cfree of OP and NP in real water samples and to study their association with humic acids and bovine albumin.

Evaluating the impacts of some environmentally relevant factors on the availability of bisphenol A with negligible-depletion SPME.

The effect of some environmentally relevant factors including salinity, pH, and humic acids on the availability of bisphenol A (BPA) was evaluated by using the negligible-depletion solid-phase microextraction (nd-SPME) biomimetic method. With the variation of salinity (0-500 mM NaCl) and pH (5.0-8.5) of aqueous solutions, the partition coefficients of BPA between the nd-SPME fiber and the aqueous solution varied in the range of logD=3.55-3.86, which indicates that the salinity and pH can influence the availability of BPA. By using Acros humic acid as model dissolved organic matter (DOM), it was also demonstrated that the environmental factors such as salinity and pH could affect the partitioning of BPA between DOM and aqueous solutions. The determined partition coefficients of BPA between dissolved organic carbon (DOC) and aqueous solutions were in the range of logD(DOC)=4.03-5.60 for Acros humic acid solutions with 1-50 mg l(-1) DOC. The influence of salinity and pH on logD(DOC) was more significant at low concentration (0-5 mg l(-1)) of DOC.

Ionic liquid for high temperature headspace liquid-phase microextraction of chlorinated anilines in environmental water samples.

Based on the non-volatility of room temperature ionic liquids (IL), 1-butyl-3-methylimidazolium hexafluorophosphate ([C4MIM][PF6]) IL was employed as an advantageous extraction solvent for high temperature headspace liquid-phase microextraction (LPME) of chloroanilines in environmental water samples. At high temperature of 90 degrees C, 4-chloroaniline, 2-chloroaniline, 3,4-dichloroaniline, and 2,4-dichloroaniline were extracted into a 10 microl drop of [C4MIM][PF6] suspended on the needle of a high-performance liquid chromatography (HPLC) microsyringe held at the headspace of the samples. Then, the IL was injected directly into the HPLC system for determination. Parameters related to LPME were optimized, and high selectivity and low detection limits of the four chlorinated anilines were obtained because the extraction was performed at high temperature in headspace mode and the very high affinity between IL and chlorinated anilines. The proposed procedure was applied for the analysis of the real samples including tap water, river water and wastewater samples from a petrochemical plant and a printworks, and only 3,4-dichloroaniline was detected in the printworks wastewater at 88.2 microg l(-1) level. The recoveries for the four chlorinated anilines in the four samples were all in the range of 81.9-99.6% at 25 microg l(-1) spiked level.

Determination of formaldehyde in shiitake mushroom by ionic liquid-based liquid-phase microextraction coupled with liquid chromatography.

Using ionic liquid as extraction solvent and 2,4-dinitrophenylhydrazine (DNPH) as derivative agent, formaldehyde in shiitake mushroom was determined by liquid-phase microextraction coupled with high-performance liquid chromatography (HPLC). Shiitake mushroom was leached with water and filtrated, then the formaldehyde in filtrate was derivatized with DNPH and extracted simultaneously into a 10mul drop of ionic liquid suspended on the tip of the microsyringe, and finally injected into the HPLC system for determination. The proposed procedure has a detection limit of 5mugl(-1) formaldehyde in extraction solution, thus the mushroom sample filtrate could be diluted with a large ratio to eliminate the influence of sample matrix. The method has a relative standard deviation of 3.5% between days for 53.5mugl(-1) formaldehyde standards. High contents of formaldehyde (119-494mugg(-1) wet weight), which is harmful for human beings, were detected in shiitake mushroom. Therefore, strategies must be taken to prevent the accumulation and strictly control the content of formaldehyde in shiitake mushroom.

Ionic liquid-based liquid-phase microextraction, a new sample enrichment procedure for liquid chromatography.

Room temperature ionic liquids (RTILs) were used as extraction solvent in liquid-phase microextraction (LPME) coupled with liquid chromatography. Using 1-hexyl-3-methylimidazolium hexafluorophosphate ([C6MIM][PF6]) as extraction solvent, some parameters related to LPME of 4-nonylphenol (4-NP) and 4-tert-octylphenol (4-t-OP) were optimized. Although [C6MIM][PF6] can suspend a much larger volume of drop on the needle of the microsyringe than the conventional solvents such as 1-octanol and carbon tetrachloride, the method sensitivity was analyte dependent because of the different partition coefficients and the relatively large viscosity of [C6MIM][PF6]. The proposed procedure has a detection limit and enrichment factor of 0.3 microg l(-1) and 163 for 4-NP, and 0.7 microg l(-1) and 130 for 4-t-OP, respectively. Aqueous samples including tap water, river water, and effluent from sewage treatment plant were analyzed by the proposed method and the recoveries at 10 microg l(-1) spiked level were in the range of 90-113%.