[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-perfor...[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-performance liquid chromatography-high resolution quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)was used to establish a fast screening method for 59 non-standard components in five categories of antiviral agents,aminoglycosides,quinolones,sulfonamides,and tetracyclines in veterinary drugs.The target drugs were separated by a Waters ACQUITY UPLC HSS T3 chromatographic column(50 mm×2.1 mm,1.8μm),and data were collected in the positive ion mode.Good separation of the 59 drugs was achieved within 7 min.[Results]In the concentration range of 0-100 ng/ml,each drug showed a good linear relationship,and the correlation coefficients were all greater than 0.999.The detection limits of the 59 drugs were in the range of 0.1-0.5 mg/ml,and the recovery under the addition concentration of 5 mg/ml was in the range of 85.2%-103.8%.[Conclusions]The method is fast,simple,accurate,and highly sensitive,and is suitable for high-throughput screening and qualitative identification of non-standard components in veterinary drug preparations.展开更多
[Objectives]This study was conducted to establish a qualitative method for rapid detection of pesticide residues in feed.[Methods]A rapid screening method for 82 pesticide residues in feed was established using ultra ...[Objectives]This study was conducted to establish a qualitative method for rapid detection of pesticide residues in feed.[Methods]A rapid screening method for 82 pesticide residues in feed was established using ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS)combined with optimized pretreatment methods.[Results]Feed samples were extracted with 0.2%formic acid-acetonitrile solution,shaken,centrifuged,and re-centrifuged,and the supernatant was filtered with a 0.22μm filter membrane for determination.The samples were separated on a Waters ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×50 mm,1.8μm),and subjected to gradient elution with methanol-water solution as the mobile phase,and scanning was performed in ESI+mode.82 compounds could be accurately qualitatively detected in 13 min.[Conclusions]This method is simple to operate,time-saving,and can be applied to rapid screening of large-scale feed.This study provides a theoretical basis for the development of new methods in the future.展开更多
基金Supported by Key R&D Project of Hebei Province(19227516D)Hebei Provincial Phase II Modern Agricultural Industry Technology System Innovation Team Building Project(HBCT2018120207)+2 种基金Hebei Provincial Phase II Modern Agricultural Industry Technology System Grass Industry Innovation Team Building Project(HBCT2018160403)Hebei Provincial Science and Technology Innovation Leading Talents(21130243A)The Fourth Batch of High-end Talent Project in Hebei Province。
文摘[Objectives]This study was conducted to provide an accurate and reliable method for rapid high-throughput screening of veterinary drug preparations.[Methods]For the matrixes of veterinary drug preparations,high-performance liquid chromatography-high resolution quadrupole time-of-flight mass spectrometry(UPLC-QTOF/MS)was used to establish a fast screening method for 59 non-standard components in five categories of antiviral agents,aminoglycosides,quinolones,sulfonamides,and tetracyclines in veterinary drugs.The target drugs were separated by a Waters ACQUITY UPLC HSS T3 chromatographic column(50 mm×2.1 mm,1.8μm),and data were collected in the positive ion mode.Good separation of the 59 drugs was achieved within 7 min.[Results]In the concentration range of 0-100 ng/ml,each drug showed a good linear relationship,and the correlation coefficients were all greater than 0.999.The detection limits of the 59 drugs were in the range of 0.1-0.5 mg/ml,and the recovery under the addition concentration of 5 mg/ml was in the range of 85.2%-103.8%.[Conclusions]The method is fast,simple,accurate,and highly sensitive,and is suitable for high-throughput screening and qualitative identification of non-standard components in veterinary drug preparations.
基金Supported by Key R&D Project in Hebei Province(19227516D)Hebei Provincial Phase II Modern Agricultural Industry Technology System Innovation Team Building Project(HBCT2018120207)+2 种基金Hebei Provincial Phase II Modern Agricultural Industry Technology System Forage Industry Innovation Team Building Project(HBCT2018160403)Tangshan Science and Technology Planning Project(21130243A)The Fourth Batch of High-end Talent Project in Hebei Province。
文摘[Objectives]This study was conducted to establish a qualitative method for rapid detection of pesticide residues in feed.[Methods]A rapid screening method for 82 pesticide residues in feed was established using ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS)combined with optimized pretreatment methods.[Results]Feed samples were extracted with 0.2%formic acid-acetonitrile solution,shaken,centrifuged,and re-centrifuged,and the supernatant was filtered with a 0.22μm filter membrane for determination.The samples were separated on a Waters ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×50 mm,1.8μm),and subjected to gradient elution with methanol-water solution as the mobile phase,and scanning was performed in ESI+mode.82 compounds could be accurately qualitatively detected in 13 min.[Conclusions]This method is simple to operate,time-saving,and can be applied to rapid screening of large-scale feed.This study provides a theoretical basis for the development of new methods in the future.