Short-Term Fermented Soybeans with Bacillus amyloliquefaciens Potentiated Insulin Secretion Capacity and Improved Gut Microbiome Diversity and Intestinal Integrity To Alleviate Asian Type 2 Diabetic Symptoms.

We determined that consuming chungkookjang fermented by Bacillus subtilis (BS) or Bacillus amyloliquefaciens (BA) alleviated hyperglycemia in partially pancreatectomized (Px) rats, an Asian type 2 diabetic (T2D) animal model. Px rats had deteriorated glucose metabolism with decreased glucose-stimulated insulin secretion and insulin sensitivity. Insulin secretion capacity was improved in the ascending order of the Px-control, positive control (3 mg of metformin/kg of body weight), BS (4.5% BS diet), BA (4.5% BA diet), and normal-control (sham-operated rats). BA and BS increased ß-cell mass and decreased malondialdehyde contents and tumor necrosis factor α expression in the islets. BA increased hepatic peroxisome proliferator-activated receptor (PPAR)-α and PPAR-ß similar to the positive control. Bacillales, Lactobacillales, and Verrucomicrobiales (Akkermensia muciniphila) increased and Enterobacteriales decreased in the BA and BS compared to the Px-control. BA prevented the decrease in the villi area and the number of goblet cells in intestinal tissues. In conclusion, BA improved glucose regulation by potentiating insulin secretion and reducing insulin resistance while maintaining gut mucin contents by improving gut microbiota in lean T2D rats.

Analysis of trace impurities in neon by a customized gas chromatography.

Excimer lasers, widely used in the semiconductor industry, are crucial for analyzing the purity of premix laser gases for the purpose of controlling stable laser output power. In this study, we designed a system for analyzing impurities in pure neon (Ne) base gas by customized GC. Impurities in pure neon (H2 and He), which cannot be analyzed at the sub-µmol/mol level using commercial GC detectors, were analyzed by a customized pulsed-discharge Ne ionization detector (PDNeD) and a pressurized injection thermal conductivity detector using Ne as the carrier gas (Pres. Inj. Ne-TCD). From the results, trace species in Ne were identified with the following detection limits: H2, 0.378µmol/mol; O2, 0.119µmol/mol; CH4, 0.880µmol/mol; CO, 0.263µmol/mol; CO2, 0.162µmol/mol (PDNeD); and He, 0.190µmol/mol (Pres. Inj. Ne-TCD). This PDNeD and pressurized injection Ne-TCD technique thus developed permit the quantification of trace impurities present in high-purity Ne.

Determination of Heterocyclic Amines and Acrylamide in Agricultural Products with Liquid Chromatography-Tandem Mass Spectrometry.

Heterocyclic amines (HCAs) and acrylamide are unintended hazardous substances generated by heating or processing of foods and are known as carcinogenic and mutagenic agents by the animal experiments. A simple method was established for a rapid and accurate determination of 12 types of HCAs (IQ, MeIQ, Glu-P-1, Glu-P-2, MeIQx, Trp-P-1, Trp-P-2, PhIP, AαC, MeAαC, Harman and Norharman) and acrylamide in three food matrices (non-fat liquid, non-fat solid and fat solid) by isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS). In every sample, a mixture of internal standards including IQ-d3, MeIQx-d3, PhIP-d3, Trp-P-2-(13)C2-(15)N and MeAαC-d3 was spiked for quantification of HCAs and (13)C3-acrylamide was also spiked for the analysis of acrylamide. HCAs and acrylamide in sample were extracted with acetonitrile and water, respectively, and then two solid-phase extraction cartridges, ChemElut: HLB for HCAs and Accucat: HLB for acrylamide, were used for efficiently removing interferences such as pigment, lipid, polar, nonpolar and ionic compounds. Established method was validated in terms of recovery, accuracy, precision, limit of detection, limit of quantitation, and linearity. This method showed good precision (RSD < 20%), accuracy (71.8~119.1%) and recovery (66.0~118.9%). The detection limits were < 3.1 ng/g for all analytes. The correlation coefficients for all the HCAs and acrylamide were > 0.995, showing excellent linearity. These methods for the detection of HCAs and acrylamide by LC-MS/MS were applied to real samples and were successfully used for quantitative monitoring in the total diet study and this can be applied to risk assessment in various food matrices.

Microwave-assisted extraction of human hair proteins.

The effectiveness of microwave-assisted extraction of proteins from human hair samples was evaluated. Extractions were performed from 2-mg hair samples in an extraction solution consisting of 25 mM Tris-HCl (pH 8.5), 2.6 M thiourea, 5 M urea, and 5% mercaptoethanol. During extraction, samples were exposed to microwave radiation (600 W) for a specified incubation period (5-120 min). The extraction efficiency of samples that had been incubated for 60 min was similar to that of samples that had been heated at 50°C for 24 h using the conventional Shindai method.

A multiresidue method for the determination of 118 pesticides in vegetable juice by gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry.

An analytical method has been developed for measuring 118 pesticides in vegetable juice. The extraction of pesticides was carried out based on dispersive solid-phase extraction, and determination was performed using gas chromatography with mass spectrometric detection (GC-MS-SIM) and liquid chromatography electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS). Pesticides were confirmed by their retention time and their quantification and identification ions by GC-MS-SIM or multiple reaction monitoring of two fragment ions by LC/ESI-MS/MS, respectively. Spiking experiments from 10 to 120 microg/kg were carried out to determine the recovery, precision, and limit of quantification (LOQ) of the method. The overall recoveries of all pesticides were between 77 and 114% with relative standard deviations lower than 14%. The LOQ for most compounds was below 5 microg/kg. The proposed method was applied successfully for the residue determination of the 118 pesticides in commercial vegetable juice samples.

A multi-residue method for the determination of 203 pesticides in rice paddies using gas chromatography/mass spectrometry.

This work reports a rapid, specific and sensitive multi-residue method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography with mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM) using one quantification ion and two identification ions for the routine analysis of 203 pesticides in rice paddies. Analyses of fortified rice paddy samples were performed at different levels (0.05, 0.20 and 0.50 mg kg(-1)). Mean recoveries from five replicates ranged from 75% to 115%, with coefficients of variation lower than 17%. The limit of quantification was in the range of 0.002-0.05 mg kg(-1) for the pesticides. 1040 rice paddy samples were analyzed for method application.

A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry.

A rapid, specific and sensitive multiresidue method based on the modified Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography with the electron impact mass spectrometric detection in the selected ion monitoring mode (GC-MS-SIM) using one target and two qualifier ions for the routine analysis of 107 pesticides in cabbage and radish has been developed. The recoveries for all the pesticides studied were from 80% to 115% with relative standard deviation lower than 15% in the concentration range of 0.030-0.360mg/kg. The limit of quantitation (LOQ) for most compounds met MRLs for pesticides in cabbage and radish in Korea. This method was successfully applied to analysis commercial cabbage and radish samples.

Determination of the strontium isotope ratio by ICP-MS ginseng as a tracer of regional origin.

This study presents the inductively coupled plasma mass spectrometry (ICP-MS) as a method for tracing the regional origin of ginseng. The results of the analysis of 15 Korean ginsengs from three different regions and of 15 Chinese ginsengs from three different regions reveal that the Sr isotope ratios (87)Sr/(86)Sr of the ginsengs differed according to their origin. For pretreatment, the ginseng samples were dried, and were dissolved through microwave digestion, then were each made to amount to 6ml with 11.9M HCl. Rb was then separated from Sr to enable an interference-free measurement through cation exchange chromatography. Six millilitres of the ginseng sample were injected in the column, and 60ml of 11.9M HCl was passed through the column at a 1mlmin(-1) flow rate to separate Rb from Sr. After Rb was eluted completely, 60ml of 5.0M HCl was passed at a 1mlmin(-1) flow rate to collect Sr. In the Sr collection step, the first 10ml portion of 30ml eluate was discarded, and the next 10ml portion was taken and was diluted with de-ionized water at a ratio of 1:3, for analysis purposes. The results of the analysis of 30 ginseng samples revealed that the Chinese ginsengs have an (87)Sr/(86)Sr ratio range of 0.672-0.701, and the Korean ginsengs 0.705-0.714. The Korean ginsengs, therefore, have a higher (87)Sr/(86)Sr ratio range than the Chinese ginsengs. Of the Korean ginsengs, (87)Sr/(86)Sr ratio range of ginsengs from Punggi, Geumsan and Hongcheon are about 0.706-0.709, 0.705-0.706, and 0.710-0.714, respectively.

A multiresidue method for the determination of 109 pesticides in rice using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography/mass spectrometry with temperature control and vacuum concentration.

A rapid, specific and sensitive multiresidue method based on the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) sample preparation method and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) has been developed for the routine analysis of 109 pesticides in rice. The method uses one quantification ion and two identification ions. Temperature control during sample preparation helps improve the recovery of thermally labile pesticides such as captan. The method was validated by the analysis of samples spiked at 0.025-0.150 mg/kg in rice matrix. The recoveries of all pesticides were between 80% and 115% with a relative standard deviation of less than 15%. The limit of quantitation (LOQ) for most compounds met the maximum residue limits (MRLs) for pesticides in rice in Korea.

Fast analysis of nicotine in tobacco using double-shot pyrolysis--gas chromatography--mass spectrometry.

A simple, rapid, and sensitive assay of nicotine in tobacco has been developed using pyrolysis-gas chromatography-mass spectrometry (DSP-GC-MS). The optimum pyrolyzer (desorption) conditions, using Korean tobacco grade B1O (0.4 mg) and n-heptadecane as an internal standard, were found to be heating from 50 to 300 degrees C at a rate of 60 degrees C/min. Replicate determinations (n = 5), on the same tobacco and using n-heptadecane as the internal standard, resulted in a nicotine content of 1.96%, with a relative standard deviation (RSD) of 1.9%. This result was in good agreement with those from established methods: the Cai ether extraction method, a chloroform extraction method, and the CORESTA recommended method. However, the DSP method requires less than half the time of the solvent extraction methods, requires less sample, is almost solvent-free, and is less labor-intensive. The DSP method was used to determine the nicotine content of eight flue-cured tobaccos from Brazil, China, Korea, and the United States, which were found to have contents ranging from 1.21 to 2.19%.

Determination of optimum conditions for the analysis of volatile components in pine needles by double-shot pyrolysis-gas chromatography-mass spectrometry.

The optimum conditions for the analysis of the volatile organic components of pine needles from Pinus densiflora using double-shot pyrolysis-gas chromatography-mass spectrometry (DSP-GC-MS) were investigated with respect to thermal desorption temperature and duration of heating. A total of 41 compounds were identified using thermal desorption temperatures of 150 degrees C, 200 degrees C, 250 degrees C and 300 degrees C. Thermal decomposition products, which include acetol, acetic acid, furfurals and phenols, were observed only at thermal desorption temperatures exceeding 250 degrees C: they were not observed in the extract from a simultaneous distillation extraction (SDE) method. Heating times of 1 s, 6 s, 30 s, 150 s and 300 s were investigated at the thermal desorption temperature of 200 degrees C, whence it was found that thermal decomposition products were produced only at heating times over 30 s. The optimum pyrolyzer conditions for the analysis of pine needles using DSP-GC-MS is 200 degrees C for 6 s. Under these conditions, this method gives comparable results to the SDE method.

Analysis of ceramides in cosmetics by reversed-phase liquid chromatography/electrospray ionization mass spectrometry with collision-induced dissociation.

A rapid, sensitive and selective method involving reversed-phase liquid chromatography (LC) with electrospray ionization (ESI) mass spectrometry (MS) was employed for determination of commercial ceramides in cosmetics for quality control of the product formulation. Using this LC/ESI-MS technique, simultaneous separation and characterization of ceramides and an impurity substance were possible. Informative fragmentation patterns were obtained by employing LC/ESI-MS in both positive and negative ionization modes to identify the structures of both sphingoid base and N-acyl chains of ceramides, and also of an impurity. The combination of positive and negative mass spectra can be used for unambiguous confirmation of ceramides and for characterization of unknown species. In-source collision-induced fragmentation resulted in characteristic product anions for the ceramides containing a phytosphingosine moiety at m/z 267, 255 and 225, and for those with a sphingosine moiety at m/z 263 and 237, regardless of the length of the fatty acyl chains. The detection limit was about 0.5 pmol in selected-ion monitoring mode. Quantification using internal standards showed good linearity and a relative standard deviation of 4%. These ceramides were more sensitively detected in positive than in negative ion mode.