Circumventing glass vial and diluent effects on solution stability of small molecule analytes during analytical method development and validation

Huang, Yande; Y, Hu; Yuill, Elizabeth M.; Marriott, Anna; Chadwick, James; Li, Jieming; Zang, Jia; Miller, Scott A.

doi:10.1016/j.jpba.2022.114676

Cited by 4 publications

(4 citation statements)

References 9 publications

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“…Glass vials are known to contain silanol active sites on their surface, which can interact with certain analytes and lead to declined recoveries. − As the FEVE completely removes the sample matrix for maximum recovery of the analytes, sample vial inertness can have substantial impacts on the recoveries. Five different brands of 2 mL sample vials were tested and compared.…”

Section: Resultsmentioning

confidence: 99%

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

Hao

Cardin

2023

Anal. Chem.

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Full evaporative vacuum extraction (FEVE) was developed in this work for analysis of a broad range of semivolatile organic compounds (SVOCs) in drinking water and surface water. Sorbent pens are used in a two-stage process that first evaporates the sample matrix through sorbent beds under vacuum to recover the lighter SVOCs, followed by the application of a higher temperature and stronger vacuum to the sample vial to recover the remaining heavier SVOCs once the matrix has evaporated. After extraction, the sorbent pens are desorbed into a GC−MS using a uniquely designed "splitless" delivery system to maximize sensitivity. Critical extraction and desorption parameters that affect the method performance were optimized. After FEVE, the sorbent pens can be stored for 7−10 days at room temperature while maintaining a less than 15% loss in analyte recovery. As a proof of concept, 10 drinking water and surface water samples were analyzed using this method. 69 analytes were detected in these water samples, with the highest concentration of 1986 ng/L for bromacil. Heptachlor epoxide, chlorpyrifos, metolachlor, butachlor, and 2,3′,4′,5-tetrachlorobiphenyl were detected in four samples. None of the analytes were above the health and safety thresholds set by California Proposition 65.

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Section: Resultsmentioning

confidence: 99%

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

Hao

Cardin

2023

Anal. Chem.

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“…The remaining barrier to this goal was the large and inconsistent variation in pH observed as a pH-adjusted stock solution of DBA was dispensed across an array of mildly alkaline borosilicate glass vials, an impact observed in other studies. 36 In order to achieve tight and reproducible control of pH, polypropylene vials were used for our studies. Full details of the automated experimental protocol can be found in the Experimental Section.…”

Section: ■ Methodologymentioning

confidence: 99%

“…Our aim was to implement a small-scale automation platform for our nitrosation experimental protocol, with the consequent advantages of being able to study many alternative sets of conditions, with parallel replicates, in a high-throughput workflow. The remaining barrier to this goal was the large and inconsistent variation in pH observed as a pH-adjusted stock solution of DBA was dispensed across an array of mildly alkaline borosilicate glass vials, an impact observed in other studies . In order to achieve tight and reproducible control of pH, polypropylene vials were used for our studies.…”

Section: Methodsmentioning

confidence: 99%

“…We were also interested in the presence of competitor amines that may be present during routine processing operations or considered species to scavenge nitrite due to preferential nitrosation. In the present study, we looked, respectively, at the effect of DBA nitrosation in the presence of equimolar quantities of the primary amine nbutylamine hydrochloride (pK a 10.72 36 ), amino acid lysine hydrochloride (pK a 10.94 37 ), and aniline hydrochloride (pK a 4.72 38 ). As can be seen from Figure 5, the rate of nitrosation of DBA appeared reduced in the presence of a competitor, but for n-butylamine and lysine, this could just be experimental noise given the similarity in pK a with the DBA conjugate acid and the very low conversions of nitrite observed.…”

Section: ■ Methodologymentioning

confidence: 99%

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Formation of N-Nitrosamines by Reaction of Secondary Dialkylamines with Trace Levels of Nitrite in Aqueous Solution: An Automated Experimental and Kinetic Modeling Study Using Di-n-butylamine

Diab,

Dominey,

Ferrini

et al. 2023

Org. Process Res. Dev.

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Healthcare marketing authorization holders are undertaking widespread risk assessment activities following the discovery of dialkyl N-nitrosamines in certain drug substances and products. A contribution to this exercise is the kinetic modeling of the reaction of secondary amines with nitrite ion in aqueous solution and identification of conditions where this would present a risk of N-nitrosamine formation. Herein, we describe automated experimental nitrosation studies on di-n-butylamine that highlight the conservative nature of the modeling approach and support the conclusion that N-nitrosamine formation only becomes a significant risk in solution at pH < 6 and at higher concentrations of nitrite. We report kinetic modeling with an updated treatment of temperature dependence and further experimentation on di-n-butylamine demonstrating our approach to be valid. Our experimentation extends to the consideration of N-nitrosamine formation from tertiary amines, which are considered less prone to nitrosation, as the mechanism includes a dealkylative step. We show a 2 orders of magnitude reduction in the rate of formation of Nnitrosodibutylamine from tributylamine compared with di-n-butylamine for the considered pH, nitrite, and amine concentrations.

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Investigation of nirmatrelvir epimerization occurred in analytical sample solution by using high resolution LC-MSn, NMR, and hydrogen/deuterium exchange study

Zheng

Wang

et al. 2023

Journal of Pharmaceutical and Biomedical Analysis

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Circumventing glass vial and diluent effects on solution stability of small molecule analytes during analytical method development and validation

Cited by 4 publications

References 9 publications

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

Full Evaporative Vacuum Extraction─A Quantitative and Green Approach for Analysis of Semivolatile Organic Compounds in Drinking Water and Surface Water Using GC–MS

Formation of N-Nitrosamines by Reaction of Secondary Dialkylamines with Trace Levels of Nitrite in Aqueous Solution: An Automated Experimental and Kinetic Modeling Study Using Di-n-butylamine

Investigation of nirmatrelvir epimerization occurred in analytical sample solution by using high resolution LC-MSn, NMR, and hydrogen/deuterium exchange study

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