Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC...Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine.展开更多
Humic acids can promote the germination of many vegetable seeds,but the key active components remain unclear.This study utilized nutrient content,cross polarization magic angle spin ^(13)C solid magnetic resonance(CPM...Humic acids can promote the germination of many vegetable seeds,but the key active components remain unclear.This study utilized nutrient content,cross polarization magic angle spin ^(13)C solid magnetic resonance(CPMAS-^(13)C-NMR)and ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS)to characterize the chemical components of humic acids.Tomato seed germination index(GI)was determined with the goal of screening the key active components of humic acids.Humic acids had a significantly higher nutrient content,except for the total nitrogen(TN)and the total phosphorus(TP)contents.Humic acids had a higher content of O-CH_(3)/NCH,aromatic C-O and carbonyl C compared to weathered coal,with significantly lower anomeric C,aromatic C and O-alkyl C/alkyl C.There were 611 different compounds identified among the test materials using UHPLC-MS.Humic acids also had a significantly higher GI(158.0%and 153.1%)than weathered coal(85.5%).The organic matter(OM),TP and available potassium(AK)contents in humic acids were significantly positively correlated with GI,and available phosphorus(AP)was significantly negatively correlated.Among the carbon components,O-CH3/NCH,aromatic C-O and O-alkyl C/alkyl C were significantly positively correlated with GI,while anomeric C was significantly negatively correlated.Furthermore,among the top 10 positive and five negative correlation compounds,lipids and lipid-like molecules[armexifolin,boviquinone 4,3-methyladipic acid,lxocarpalactone A,monic acid,DG(20:1(11Z)/18:4(6Z,9Z,12Z,15Z)/0:0),and brassinolide]and organic acids and derivatives(N-acetylglutamic acid,8-hydroxy-5,6-octadienoic acid,acetyl-L-tyrosine,and hydroxyprolyl-methionine)in humic acids might be crucial active components for improving tomato seed germination.The results provided direct evidence for the identification of bioactive molecules of humic acids,and a scientific basis for the precise utilization of bioactive molecular components of humic acids in sustainable agricultural development.展开更多
Douchi is a kind of traditional Chinese fermented soybean food.Ultra-high performance liquid chromatography quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS)was applied to separate and identify 12 kinds of iso...Douchi is a kind of traditional Chinese fermented soybean food.Ultra-high performance liquid chromatography quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS)was applied to separate and identify 12 kinds of isoflavones in Douchi within 16 min.The chromatographic separation was carried out on an ACQUITY UPLC HSS T3 column with a gradient elution program where water containing 0.1%formic acid and acetonitrile containing 0.1%formic acid were used as mobile phases.Detection by using electrospray ionization of positive ion mode was applied in the mass spectrometry.Isoflavones were identified by determining the accurate mass and referring to references in this study.展开更多
文摘Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine.
基金Supported by the National Natural Science Foundation of China(42207371)the Technological Project of Jiangsu Vocational College of Agriculture and Forestry(2021kj17)+1 种基金Yafu Technology Innovation and Service Major Project of Jiangsu Vocational College of Agriculture and Forestry(2024kj01)Key Research Projects of Jiangsu Vocational College of Agriculture and Forestry(2023kj14)。
文摘Humic acids can promote the germination of many vegetable seeds,but the key active components remain unclear.This study utilized nutrient content,cross polarization magic angle spin ^(13)C solid magnetic resonance(CPMAS-^(13)C-NMR)and ultra-high performance liquid chromatography-mass spectrometry(UHPLC-MS)to characterize the chemical components of humic acids.Tomato seed germination index(GI)was determined with the goal of screening the key active components of humic acids.Humic acids had a significantly higher nutrient content,except for the total nitrogen(TN)and the total phosphorus(TP)contents.Humic acids had a higher content of O-CH_(3)/NCH,aromatic C-O and carbonyl C compared to weathered coal,with significantly lower anomeric C,aromatic C and O-alkyl C/alkyl C.There were 611 different compounds identified among the test materials using UHPLC-MS.Humic acids also had a significantly higher GI(158.0%and 153.1%)than weathered coal(85.5%).The organic matter(OM),TP and available potassium(AK)contents in humic acids were significantly positively correlated with GI,and available phosphorus(AP)was significantly negatively correlated.Among the carbon components,O-CH3/NCH,aromatic C-O and O-alkyl C/alkyl C were significantly positively correlated with GI,while anomeric C was significantly negatively correlated.Furthermore,among the top 10 positive and five negative correlation compounds,lipids and lipid-like molecules[armexifolin,boviquinone 4,3-methyladipic acid,lxocarpalactone A,monic acid,DG(20:1(11Z)/18:4(6Z,9Z,12Z,15Z)/0:0),and brassinolide]and organic acids and derivatives(N-acetylglutamic acid,8-hydroxy-5,6-octadienoic acid,acetyl-L-tyrosine,and hydroxyprolyl-methionine)in humic acids might be crucial active components for improving tomato seed germination.The results provided direct evidence for the identification of bioactive molecules of humic acids,and a scientific basis for the precise utilization of bioactive molecular components of humic acids in sustainable agricultural development.
基金Supported by the Youth Fund Project from Beijing Academy of Agricultural and Forestry Sciences(QNJJ202001)。
文摘Douchi is a kind of traditional Chinese fermented soybean food.Ultra-high performance liquid chromatography quadrupole-time of flight mass spectrometry(UPLC-QTOF-MS)was applied to separate and identify 12 kinds of isoflavones in Douchi within 16 min.The chromatographic separation was carried out on an ACQUITY UPLC HSS T3 column with a gradient elution program where water containing 0.1%formic acid and acetonitrile containing 0.1%formic acid were used as mobile phases.Detection by using electrospray ionization of positive ion mode was applied in the mass spectrometry.Isoflavones were identified by determining the accurate mass and referring to references in this study.
