Chiral determination of nornicotine, anatabine and anabasine in tobacco by achiral gas chromatography with (1S)-(-)-camphanic chloride derivatization: Application to enantiomeric profiling of cultivars and curing processes

Cai, Kai; Zhao, Huina; Yin, Runsheng; Lin, Yechun; Lei, Bo; Wang, Anping; Pan, Wenjie; Cai, Baochang; Gao, Weichang; Wang, Feng

doi:10.1016/j.chroma.2020.461361

Cited by 7 publications

(4 citation statements)

References 35 publications

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“…The matrix effects were calculated using the following equation: matrix effect % = {[(matrix-blank)/water] × 100}, where [matrix] is the measured value in the spiked extraction solution, [blank] is the measured value in the non-spiked extraction solution, and [water] is the measured value in the spiked water. A matrix effect of 100% means that no matrix effects are present, while a ratio above or below 100% means matrix enhancement effect or suppression effect, respectively . The matrix effect was evaluated with an extraction solution before and after purification with CARB SPE.…”

Section: Resultsmentioning

confidence: 99%

“…A matrix effect of 100% means that no matrix effects are present, while a ratio above or below 100% means matrix enhancement effect or suppression effect, respectively. 37 The matrix effect was evaluated with an extraction solution before and after purification with CARB SPE. The experimental results showed that the matrix effect before purification was a significant suppression effect with a ratio of 72.5%, while the matrix effect after purification was a slight suppression effect with a ratio of 98.6%.…”

Section: Resultsmentioning

confidence: 99%

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Development and Application of Portable Reflectometric Spectroscopy Combined with Solid-Phase Extraction for Determination of Potassium in Flue-Cured Tobacco Leaves

Cai

Gao

et al. 2023

ACS Omega

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Potassium (K) plays important roles in the energy and substance conversion of tobacco metabolism and is also regarded as one of the important indicators of tobacco quality evaluation. However, the K quantitative analytical method shows poor performance in terms of being easy-to-use, cost-effective, and portable. Here, we developed a rapid and simple method for the determination of K content in flue-cured tobacco leaves, including water extraction with 100 °C heating, purification with solid-phase extraction (SPE), and analysis with portable reflectometric spectroscopy based on K test strips. The method development consisted of optimization of the extraction and test strip reaction conditions, screening of SPE sorbent materials, and evaluation of the matrix effect. Under the optimum conditions, good linearity was observed in 0.20–0.90 mg/mL with a correlation coefficient >0.999. The extraction recoveries were found to be in the range of 98.0–99.5% with a repeatability and reproducibility of 1.15–1.98% and 2.04–3.26%, respectively. The sample measured range was calculated to be 0.76–3.68% K. Excellent agreement was found in accuracy between the developed reflectometric spectroscopy method and the standard method. The developed method was applied to analyze the K content in different cultivars, and the content varied greatly among the samples with lowest and highest contents for Y28 and Guiyan 5 cultivars, respectively. This study can provide a reliable approach for K analysis, which may become available on-site in a quick on-farm test.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Development and Application of Portable Reflectometric Spectroscopy Combined with Solid-Phase Extraction for Determination of Potassium in Flue-Cured Tobacco Leaves

Cai

Gao

et al. 2023

ACS Omega

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“…To further improve hydrolysis efficiency, a multivariate strategy based on the response surface methodology with a four-factor, three-level BBD was further employed to optimize important ultrasonic acid hydrolysis conditions, such as liquid-to-material ratio/ v/w (A), ultrasonic intensity power/W (B), hydrolysis temperature/°C (C), and time/min (D). BBD is a class of rotatable or nearly rotatable second-order designs based on combinations of three levels [ 30 ]. The advantage is that it is more efficient, convenient, and less expensive with no axial points [ 31 ].…”

Section: Resultsmentioning

confidence: 99%

“…The developed method was validated with parameters of linearity (internal standard calibration curve), sensitivity (limits of detection (LODs) and limits of quantification (LOQs)), stability, accuracy (extraction recovery), and precision (repeatability and reproducibility) under optimum conditions [ 30 ]. For linearity, the diamines standard solutions and internal standards were subjected to 2M HCl/acetonitrile ( v/v = 1:1) for derivatization and extraction procedures described above ( Section 3.4 ).…”

Section: Resultsmentioning

confidence: 99%

Determination of Residual Diisocyanates and Related Diamines in Biodegradable Mulch Films Using N-Ethoxycarbonylation Derivatization and GC-MS

Cai¹,

Lin²,

Ma³

et al. 2022

Molecules

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Diisocyanates are highly reactive compounds with two functional isocyanate groups. The exposure of diisocyanates is associated with severely adverse health effects, such as asthma, inflammation in the respiratory tract, and cancer. The hydrolysis product from diisocyanates to related diamines is also a potential carcinogen. Here, we developed an effective, accurate, and precise method for simultaneous determination of residual diisocyanates and related diamines in biodegradable mulch films, based on N-ethoxycarbonylation derivatization and gas chromatography-mass spectrometry. The method development included the optimization of ultrasonic hydrolysis and extraction, screening of N-ethoxycarbonylation conditions with ethyl chloroformate, evaluation of the diamines degradation, and analysis of the fragmentation mechanisms. Under the optimum experimental conditions, good linearity was observed with R2 > 0.999. The extraction recoveries were found in the range of 93.9–101.2% with repeatabilities and reproducibilities in 0.89–8.12% and 2.12–10.56%, respectively. The limits of detection ranged from 0.0025 to 0.057 µg/mL. The developed method was applied to commercial polybutylene adipate co-terephthalate (PBAT) biodegradable mulch film samples for analysis of the diverse residual diisocyanates and related diamine additives. The components varied greatly among the sample from different origin. Overall, this study provides a reliable method for assessing safety in biodegradable mulch films.

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Enantiomeric Analysis of Chiral Drugs Using Mass Spectrometric Methods: A Comprehensive Review

Vallamkonda,

Sethi,

Satti

et al. 2024

Chirality

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Chirality plays a crucial role in the drug development process, influencing fundamental chemical and biochemical processes and significantly affecting our daily lives. This review provides a comprehensive examination of mass spectrometric (MS) methods for the enantiomeric analysis of chiral drugs. It thoroughly investigates MS‐hyphenated techniques, emphasizing their critical role in achieving enantioselective analysis. Furthermore, it delves into the intricate chiral recognition mechanisms inherent in MS, elucidating the fundamental principles that govern successful chiral separations. By critically assessing the obstacles and potential benefits associated with each MS‐based method, this review offers valuable insights for researchers navigating the complexities of chiral analysis. Both qualitative and quantitative approaches are explored, presenting a comparative analysis of their strengths and limitations. This review is aimed at significantly enhancing the understanding of chiral MS methods, serving as a crucial resource for researchers and practitioners engaged in enantioselective studies.

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Chiral determination of nornicotine, anatabine and anabasine in tobacco by achiral gas chromatography with (1S)-(-)-camphanic chloride derivatization: Application to enantiomeric profiling of cultivars and curing processes

Cited by 7 publications

References 35 publications

Development and Application of Portable Reflectometric Spectroscopy Combined with Solid-Phase Extraction for Determination of Potassium in Flue-Cured Tobacco Leaves

Development and Application of Portable Reflectometric Spectroscopy Combined with Solid-Phase Extraction for Determination of Potassium in Flue-Cured Tobacco Leaves

Determination of Residual Diisocyanates and Related Diamines in Biodegradable Mulch Films Using N-Ethoxycarbonylation Derivatization and GC-MS

Enantiomeric Analysis of Chiral Drugs Using Mass Spectrometric Methods: A Comprehensive Review

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