“…Overall, the precision data were similar to other studies with similar and different methodologies (Campanella et al ; Bosch et al ; Armenta et al ; Azilawati et al ; Seow et al ), demonstrating the high precision, repeatability, and reproducibility of the UPLC system with this invertebrate matrix. The precision values reported here for CYA and MSO were also similar to the < 9% RSD reported in Thera et al () for both retention time and peak area, using a 25 pmol μ L −1 spiked unoxidized zooplankton hydrolysate. The precision of the method over time was reliable with a mean CV of 6.8% for samples (excluding PHE and TYR; Supporting Information Table S1), similar to data in the literature (e.g., Armenta et al ).…”
Section: Assessment and Discussionsupporting
confidence: 89%
“…SER is partially destroyed with hydrolysis (Rutherfurd and Gilani ) and because connective tissue is rich in THR and SER, homogeneity of samples is critical to reduce variability in these amino acids. The variability of CYA and MSO in the invertebrate matrix was consistent with other matrices in the literature (Bosch et al ; Rutherfurd et al ; Thera et al ). Normalizing to the percent of TAAs had the greatest impact on the algae replicates; as absolute concentrations, the RPDs for almost all amino acids were > 15% (Table ), while as relative concentrations no amino acids had a median RPD > 15%, with many amino acids < 5% (excluding TYR and PHE) (Fig.…”
Section: Assessment and Discussionsupporting
confidence: 89%
“…The objective of the present study was to evaluate the AccQ·Tag ultra ultra‐high performance liquid chromatography (UPLC) method (Boogers et al ) using PFA oxidation to quantify the amino acid (including thiols) composition of invertebrates, fish, and algae as no such evaluation currently exists. Method validation studies for the UPLC to date exclude any analysis of cysteine and methionine (Boogers et al ; Armenta et al ) or PFA oxidation was not performed (Thera et al ). A rigorous method is especially needed for measurements of sulfur amino acids, as their abundance in freshwater biota is not well understood, nor is their role in the fate of methylmercury in aquatic food webs.…”
Thiol amino acids in proteins store metals like mercury, but established methods for their quantitation in freshwater species have had limited application and evaluation. As such, literature on the amino acid composition of aquatic species often lacks the thiols cysteine and methionine. Here, we evaluated a performic acid (PFA) oxidation method to determine its suitability to measure cysteine and methionine, as well as 15 other amino acids, in novel matrices (zooplankton, benthic invertebrates, fishes, and algae). Protein-bound amino acids were oxidized with PFA, hydrolyzed in hydrochloric acid, derivatized with AccQÁTag ultra (Waters), and separated by ultra-high performance liquid chromatography with fluorescence detection. PFA oxidation was successful in determining precise results for 15 amino acids, including the sulfur amino acids, with the complete loss of tyrosine (TYR) and poor precision of phenylalanine (PHE). The overall variability of the method was 11% (excluding TYR and PHE), or 6% when reported as relative percentages, comparable to methods without PFA oxidation in other matrices. Except for TYR and thiols, PFA oxidation did not affect the amino acid composition of these biota. Overall, the findings were reproducible and comparable to other approaches and suggest this is a rigorous method for measuring sulfur amino acids and the overall amino acid composition for aquatic biota, both of which are rare in the literature.
“…Overall, the precision data were similar to other studies with similar and different methodologies (Campanella et al ; Bosch et al ; Armenta et al ; Azilawati et al ; Seow et al ), demonstrating the high precision, repeatability, and reproducibility of the UPLC system with this invertebrate matrix. The precision values reported here for CYA and MSO were also similar to the < 9% RSD reported in Thera et al () for both retention time and peak area, using a 25 pmol μ L −1 spiked unoxidized zooplankton hydrolysate. The precision of the method over time was reliable with a mean CV of 6.8% for samples (excluding PHE and TYR; Supporting Information Table S1), similar to data in the literature (e.g., Armenta et al ).…”
Section: Assessment and Discussionsupporting
confidence: 89%
“…SER is partially destroyed with hydrolysis (Rutherfurd and Gilani ) and because connective tissue is rich in THR and SER, homogeneity of samples is critical to reduce variability in these amino acids. The variability of CYA and MSO in the invertebrate matrix was consistent with other matrices in the literature (Bosch et al ; Rutherfurd et al ; Thera et al ). Normalizing to the percent of TAAs had the greatest impact on the algae replicates; as absolute concentrations, the RPDs for almost all amino acids were > 15% (Table ), while as relative concentrations no amino acids had a median RPD > 15%, with many amino acids < 5% (excluding TYR and PHE) (Fig.…”
Section: Assessment and Discussionsupporting
confidence: 89%
“…The objective of the present study was to evaluate the AccQ·Tag ultra ultra‐high performance liquid chromatography (UPLC) method (Boogers et al ) using PFA oxidation to quantify the amino acid (including thiols) composition of invertebrates, fish, and algae as no such evaluation currently exists. Method validation studies for the UPLC to date exclude any analysis of cysteine and methionine (Boogers et al ; Armenta et al ) or PFA oxidation was not performed (Thera et al ). A rigorous method is especially needed for measurements of sulfur amino acids, as their abundance in freshwater biota is not well understood, nor is their role in the fate of methylmercury in aquatic food webs.…”
Thiol amino acids in proteins store metals like mercury, but established methods for their quantitation in freshwater species have had limited application and evaluation. As such, literature on the amino acid composition of aquatic species often lacks the thiols cysteine and methionine. Here, we evaluated a performic acid (PFA) oxidation method to determine its suitability to measure cysteine and methionine, as well as 15 other amino acids, in novel matrices (zooplankton, benthic invertebrates, fishes, and algae). Protein-bound amino acids were oxidized with PFA, hydrolyzed in hydrochloric acid, derivatized with AccQÁTag ultra (Waters), and separated by ultra-high performance liquid chromatography with fluorescence detection. PFA oxidation was successful in determining precise results for 15 amino acids, including the sulfur amino acids, with the complete loss of tyrosine (TYR) and poor precision of phenylalanine (PHE). The overall variability of the method was 11% (excluding TYR and PHE), or 6% when reported as relative percentages, comparable to methods without PFA oxidation in other matrices. Except for TYR and thiols, PFA oxidation did not affect the amino acid composition of these biota. Overall, the findings were reproducible and comparable to other approaches and suggest this is a rigorous method for measuring sulfur amino acids and the overall amino acid composition for aquatic biota, both of which are rare in the literature.
Aniline and its derivatives, as the basic aromatic amine compounds, are widely used in different fields such as chemistry, biology, medicine, dyes, polymer materials and agriculture. Moreover, hydrogenation reduction of nitrobenzene is a simple method for the synthesis of aniline. According to the difference of proton/electron donor, the reduction of nitrobenzene can be divided into Bechamp reduction, catalytic hydrogenation, catalytic hydrogen transfer and Zinin reduction. Zinin reduction is a method for preparing aniline by reducing nitro group by using sulfide as electron donor and protic solvent as hydrogen source, which is widely used in the laboratory research and industrial production. In this review, Zinin reduction method is systematically summarized. The principle of reduction of nitro group by sulfide is clarified from the types of sulfide reductants, the reduction mechanism of nitro group, and the application of nitro group reduction. Additionally, the reduction mechanism of nitro group by elemental sulfur, sulfide, polysulfide and hydrosulfide is detailly elucidated, and the regulatory mechanism of OH and H2O in the reduction of nitro group by sulfide is explained in detail. Finally, the ability and application effect of different sulfides as reductants to reduce nitro group are analyzed in terms of atom economy.
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