The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, whi...The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, which is based on a data-dependent acquisition of isotope ions and result verified by full scan mass spectrum. The distinguished advantage of data-dependent scan is rapidness because it requires minimum sample preparation, and all the necessary data can be obtained in one chromatographic run. In addition, it is highly sensitive and selective, allowing detection of trace metabolites even in the presence of complex biomatrix. As a result, four phase-Ⅰ（M1--M4） and four Phase-Ⅱ（M5--M8） metabolites of brodimoprim were identified in urine after the oral administration of hrodimoprim to Wistar rats. Their chemical structures were proposed based on the interpretation of their CID fragmentation characterizations and the metabolic pathway was exhibited in this article.展开更多
Thiophonate-methyl(TPM) is one of fungicides and pesticides widely used in agriculture field.However,the residue of its benzimidazole(BZD) metabolites in related agricultural products poses a potential risk to consume...Thiophonate-methyl(TPM) is one of fungicides and pesticides widely used in agriculture field.However,the residue of its benzimidazole(BZD) metabolites in related agricultural products poses a potential risk to consumers.In this paper,nickel oxide nanoparticle-deposited silica(SiO_2@NiO) composite was used for the selective enrichment and purification of TPM's BZD metabolites in celery cabbage sprayed with TPM.Meanwhile,high-performance liquid chromatography coupled with precursor ion scan-mass spectrometry(HPLC-PIS-MS) and high-resolution MS/MS analysis(HR-MS/MS) was utilized for their qualitative and quantitative analysis.Twenty-one potential TPM's BZD metabolites were found and four of them were identified.One metabolite was discovered for the first time.Besides,a robust and sensitive quantitative method was developed with good linearities(R^2> 0.9972) within a wide range of 10.00-1000 ng/g.The detection limits of three known TPM's metabolites were within the range of 3.20-4.90 ng/g.Relative standard deviations(RSDs) of intra-day and inter-day precisions were less than 18.3%,which showed perfect reproducibility.The method was successfully applied to monitoring TPM's BZD metabolites in celery cabbage sprayed with TPM and the concentration versus time curves of TPM's metabolites in celery cabbage were plotted.This method is expected to be used to monitor BZD residues in various fruits and vegetables.展开更多
基金the National Natural Science Foundation of China(Nos.30630075 and 20675056)Natural Science Founda-tion of Tianjin City,China(No.07JCYBJC01600)
文摘The present article covers a simple approach to detect and subsequently identify in vivo metabolites of brodimoprim, using high performance liquid chromatography coupled to ion trap mass spectrometer（LC/ESI-MS）, which is based on a data-dependent acquisition of isotope ions and result verified by full scan mass spectrum. The distinguished advantage of data-dependent scan is rapidness because it requires minimum sample preparation, and all the necessary data can be obtained in one chromatographic run. In addition, it is highly sensitive and selective, allowing detection of trace metabolites even in the presence of complex biomatrix. As a result, four phase-Ⅰ（M1--M4） and four Phase-Ⅱ（M5--M8） metabolites of brodimoprim were identified in urine after the oral administration of hrodimoprim to Wistar rats. Their chemical structures were proposed based on the interpretation of their CID fragmentation characterizations and the metabolic pathway was exhibited in this article.
基金The National Natural Science Foundation of China(No.31671929,21635006 and 31670373)supported this work。
文摘Thiophonate-methyl(TPM) is one of fungicides and pesticides widely used in agriculture field.However,the residue of its benzimidazole(BZD) metabolites in related agricultural products poses a potential risk to consumers.In this paper,nickel oxide nanoparticle-deposited silica(SiO_2@NiO) composite was used for the selective enrichment and purification of TPM's BZD metabolites in celery cabbage sprayed with TPM.Meanwhile,high-performance liquid chromatography coupled with precursor ion scan-mass spectrometry(HPLC-PIS-MS) and high-resolution MS/MS analysis(HR-MS/MS) was utilized for their qualitative and quantitative analysis.Twenty-one potential TPM's BZD metabolites were found and four of them were identified.One metabolite was discovered for the first time.Besides,a robust and sensitive quantitative method was developed with good linearities(R^2> 0.9972) within a wide range of 10.00-1000 ng/g.The detection limits of three known TPM's metabolites were within the range of 3.20-4.90 ng/g.Relative standard deviations(RSDs) of intra-day and inter-day precisions were less than 18.3%,which showed perfect reproducibility.The method was successfully applied to monitoring TPM's BZD metabolites in celery cabbage sprayed with TPM and the concentration versus time curves of TPM's metabolites in celery cabbage were plotted.This method is expected to be used to monitor BZD residues in various fruits and vegetables.
