[Determination of trace -amanitin in urine of mushroom poisoning patient by online solid phase extraction-liquid chromatography-tandem mass spectrometry].

An analytical method was established for the determination of trace -amanitin in the urine of patients suffering from mushroom poisoning by online solid phase extraction-liquid chromatography-tandem mass spectrometry (online SPE-LC-MS/MS). The sample was protein precipitated with formic acid acidified acetonitrile-methanol (5:1, v/v). Reversed-phase liquid-liquid microextraction was used to remove the organic solvent from the sample extract.

Health risk assessment of heavy metals in marine fish to the population in Zhejiang, China.

Environmental pollution with toxic metals can lead to the possible contamination of the marine fish. We investigated the levels of As, Cd, Cr, Hg and Pb in 652 marine fish samples (15 species) collected from coastal areas of Zhejiang, China and estimated their health risk. Mean concentrations of As, Cd, Cr, Hg and Pb were 0.

[Analysis of multi-minerals in seafoods in Zhejiang Province].

Objective: To analyze the contents of Ca, K, Na, Mg, Fe, Zn, Cu and Mn in 33 kinds of marine products, such as fish, shrimp, crab, shellfish and mollusk.

Methods: The national standard GB 5009. 268-2016 Determination of multi elements in foods was used for determination.

[Eight vitamin E congeners in seafood and aquatic products in Zhejiang Province].

Objective: Comparison and analysis of α-, β-, γ-, δ-tocopherol(T) and α-, β-, γ-, δ-tocotrienol(T3) in 44 species of seafood and aquatic products is under processed to enrich the database of food composition in China and provide a scientific reference for dietary intake choice.

Methods: Quantitative and correlation analysis of eight vitamin E isomers were based on external calibration method with reversed-phase high-performance liquid chromatography-fluorescence detector, after hot saponification with alkaline and liquid-liquid extraction.

Results: The content of α-tocopherol equivalent(α-TE) in seafood and aquatic products varied greatly(from 0.

[Fat-soluble vitamins in different eggs and egg products in Hangzhou City].

Objective: To analyze the contents of fat-soluble vitamins in different kinds of eggs and egg products in Hangzhou City.

Methods: The contents of fat-soluble vitamin A, vitamin E, vitamin K_1 and vitamin K_2(menaquinone-4, menaquinone-7 and menaquinone-9) in eggs and egg products were determined by the high-performance liquid chromatography method. The contents of vitamin D were determined by high performance liquid chromatography-tandem mass spectrometry.

Determination of ibotenic acid and muscimol in plasma by liquid chromatography-triple quadrupole mass spectrometry with bimolecular dansylation.

Ibotenic acid (IBA) is an amino acid and muscimol (MUS) is the decarboxyl derivative of IBA. They are mushroom neurotoxins with high polarity and low molecular weight. Only one transition (159->113 for IBA and 115->98 for MUS) can be found when directly measured by high performance liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS).

Screening of multi-class antibiotics in pork meat by LC-Orbitrap-MS with modified QuEChERS extraction.

The quantification capability of high resolution mass spectrometry is of great interest to analysts. We described a method for analysis of multi-class antibiotics in pork meat by UPLC-quadrupole (Q)-Orbitrap-MS. The QuEChERS approach with a clean-up step using a sorbent of primary-secondary amine (PSA) and C18 was adopted for sample preparation, and 37 antibiotics including beta-lactams, tetracyclines, sulfonamides, fluoroquinolones and macrolides were analyzed.

[Determination of vitamin K in animal foods].

Objective: To establish a high performance liquid chromatography method with fluorescence detection for a variety of vitamin K and to assess the content of vitamin K in animal foods.

Methods: Animal foods were hydrolyzed by 0.2 g lipase and 0.

Simultaneous detection of multiple hydroxylated polychlorinated biphenyls from biological samples using ultra-high-performance liquid chromatography with isotope dilution tandem mass spectrometry.

We established a method for the separation and detection of nine hydroxylated polychlorinated biphenyls in whole blood and urine samples using ultra high performance liquid chromatography coupled with electrospray negative ionization tandem mass spectrometry. Clean-up procedures involved a filtration step, and optimization involved a pretreatment step consisting of a simple liquid-liquid extraction using hydrated silica-gel chromatography (5%). Nine hydroxylated polychlorinated biphenyls were separated on an ultra high performance liquid chromatography HSS T3 column using a gradient elution program of 2 mmol ammonium formate aqueous solution (A) and methanol (B).

A feasibility study of producing a peanut oil matrix candidate reference material and its application to support monitoring of aflatoxins statues for public health purposes.

The first peanut oil reference materials in naturally contaminated aflatoxins was developed, because of the high consumption of this product and the potential risk associated herewith. Based on liquid chromatographic method, homogeneity, short-term of 60 °C for seven days and long-term of 25 °C for twelve months' stability studies of candidates were assessed. The obtained data and statistical results showed a successful feasibility study, without any significant trend.

Authentication of pork in meat mixtures using PRM mass spectrometry of myosin peptides.

Adulteration of meat products is a major concern not only for economic fraud, but also for ethical reasons. In this study, we presented a parallel reaction monitoring (PRM) mass spectrometry approach for detection of trace pork in meat mixtures (chicken, sheep, and beef). Specific peptides were identified and screened by a shotgun proteomic approach based on tryptic digests of certain protein.

Distribution of metals and metalloids in dried seaweeds and health risk to population in southeastern China.

Concern about metals and metalloids, especially heavy metals in seaweeds has risen due to potential health risk. This study investigated the distribution of 10 metals and metalloids in 295 dried seaweeds (brown and red) and estimated the possible health risk via hazard index (HI). Elements in seaweeds can be sequenced in descending order by mean values: Al > Mn > As > Cu > Cr > Ni > Cd > Se > Pb > Hg.

Fast and quantitative determination of saxitoxin and neosaxitoxin in urine by ultra performance liquid chromatography-triple quadrupole mass spectrometry based on the cleanup of solid phase extraction with hydrophilic interaction mechanism.

Saxitoxin (STX) and neosaxitoxin (NEO) are water-soluble toxins and their cleanup in bio-matrix is a hot topic but difficult problem. A fast and quantitative determination method for STX and NEO in urine was developed using ultra performance liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) based on the cleanup of solid phase extraction (SPE) with hydrophilic interaction (HILIC) mechanism. Acetonitrile/methanol/water mixture was used to extract the toxins in urine.

[Determination of amanitins and phallotoxins in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry].

A fast and wide linear range method was established for the determination of mushroom toxins amanitins (-amanitin,-amanitin and -amanitin) and phallotoxins (phallacidin and phalloidin) in wild mushrooms by online liquid chromatography-diode array detector-tandem mass spectrometry (LC-DAD-MS/MS). The mushroom toxins were extracted with methanol, and diluted with water. The extracts were separated on an XBridge BEH C column (150 mm×3.

Simultaneous determination of five Alternaria toxins in cereals using QuEChERS-based methodology.

Two analytical approaches, including ultra-high performance liquid chromatograph linked with photo-diode array/fluorescence detector, and ultra-high performance liquid chromatography-tandem mass spectrometry, have been proposed for simultaneous determination of five Alternaria toxins in cereals, which both based on QuEChERS strategy. After QuEChERS extraction and salting out, the collected supernatant was subjected to an extra dispersive liquid-liquid microextraction step prior to quantitative analysis. Response surface methodology based on central composite design was employed to optimize the micro-extraction conditions.

Quantification of 16 β-lactams in chicken muscle by QuEChERS extraction and UPLC-Q-Orbitrap-MS with parallel reaction monitoring.

A method is described for the analysis of 16 β-lactams in chicken muscle by UPLC-quadrupole(Q)-Orbitrap-MS with parallel reaction monitoring (PRM). QuEChERS approach includes clean-up step by sorbent of primary-secondary amine (PSA) and C18 was adopted for sample preparation. Q-Orbitrap with PRM showed high sensitivity with limits of detection (LODs) ranged from 0.

High-performance liquid chromatographic determination of multi-mycotoxin in cereals and bean foodstuffs using interference-removal solid-phase extraction combined with optimized dispersive liquid-liquid microextraction.

A novel pre-treatment was proposed for the simultaneous determination of aflatoxins, ochratoxin A and zearalenone in foodstuffs using high-performance liquid chromatography with fluorescence detection. The analytical procedure was based on a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure, followed by salting out and purification with a C solid-phase extraction column as interference removal clean-up. Subsequently, collected supernatant was subjected to dispersive liquid-liquid microextraction.

Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection.

A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.

Study of the matrix effects of tetrodotoxin and its content in cooked seafood by liquid chromatography with triple quadrupole mass spectrometry.

Tetrodotoxin is a marine biotoxin with high acute toxicity. The levels in cooked seafood will help us to assess its intake in humans and may help assess the risk of toxicity. However, heavy matrices hinder the direct quantitation of tetrodotoxin.

A combined tryptic peptide and winged peptide internal standard approach for the determination of α-lactalbumin in dairy products by ultra high performance liquid chromatography with tandem mass spectrometry.

A robust ultra high performance liquid chromatography with tandem mass spectrometry method at peptide level was established for measuring α-lactalbumin in various dairy products. An isotope-labeled winged peptide (VKKILDKVG*INYW*LAHKALCSEKL) with extra amino acids of the sequence of signature peptide concatenated at each end as the internal standard was spiked in samples to participate in the whole tryptic digestion process. The peptide VG*INYW*LAHK that resulted from the isotope-labeled winged peptide was used as the final isotopically labeled internal standard of the α-lactalbumin signature peptide (VGINYWLAHK) during the quantitative analysis.

Determination of bovine lactoferrin in dairy products by ultra-high performance liquid chromatography-tandem mass spectrometry based on tryptic signature peptides employing an isotope-labeled winged peptide as internal standard.

A new and sensitive determination method was developed for bovine lactoferrin in dairy products including infant formulas based on the signature peptide by ultra high-performance liquid chromatography and triple-quadrupole tandem mass spectrometry under the multiple reaction monitoring mode. The simple pretreatment procedures included the addition of a winged peptide containing the isotope-labeled signature peptide as internal standard, followed by an enzymatic digestion with trypsin. The signature peptide was chosen and identified from the tryptic hydrolyzates of bovine lactoferrin by ultra high-performance liquid chromatography and quadrupole-time-of-flight tandem mass spectrometry based on sequence database search.

[Simultaneous determination of ethyl carbamate and chloropropanols in flavorings by gas chromatography-triple quadrupole tandem mass spectrometry].

A simultaneous determination method for ethyl carbamate (EC) and chloropropanols (3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD)) in flavorings was developed by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). After spiked with internal standard, the sample was extracted by matrix solid-phase dispersion extraction technique with an Extrelut NT column. Hexane was used to wash the fat soluble matrix interferences and then an ethyl acetate-ethyl ether (20: 80, v/v) mixture was added to elute the analytes.

Simultaneous determination of 3-monochloropropane-1,2-diol and acrylamide in food by gas chromatography-triple quadrupole mass spectrometry with coupled column separation.

Both 3-monochloropropane-1,2-diol (3-MCPD) and acrylamide are contaminants found in heat-processed foods and their related products. A quantitative method was developed for the simultaneous determination of both contaminants in food by gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). The analytes were purified and extracted by the matrix solid-phase dispersion extraction (MSPDE) technique with Extrelut NT.

Determination of disialoganglioside GD3 and monosialoganglioside GM3 in infant formulas and whey protein concentrates by ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry.

A method of ultra-performance liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry (UPLC-ESI-MS/MS) has been established for simultaneous determination of major disialoganglioside 3 (GD3) and monosialoganglioside 3 (GM3) in infant formulas and whey protein concentrates. Gangliosides were extracted by using the technique of Svennerholm and Fredman and then cleaned up with OASIS HLB solid-phase extraction (SPE) cartridges. The various molecular species of gangliosides were separated on an Acquity UPLC BEH C8 column and analyzed under the negative ion mode.