JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2023
·
IF 3
Hong Yang,Jing Wang,Wenming Cao
Tetramethylpyrazine (TMP) is an important bioactive compound in vinegars, contributing to their health-enhancing attributes. It serves as a crucial benchmark for the assessment of vinegar quality. Unfortunately, inaccuracies have arisen due to incomplete extraction techniques and the use of an inappropriate standard substance. These challenges have significantly curtailed comprehensive exploration into the underlying TMP formation mechanisms, impeding advancements within prevailing benchmarks and methodologies governing vinegar products. To address these challenges, several critical parameters, encompassing pH, solvent type, centrifugal force, extraction times and reference materials were investigated and optimized. The TMP content was determined by adjusting the pH to 9 using a sodium hydroxide solution, followed by extraction with ethyl acetate and subsequent re-extraction of the ethyl acetate layer with 0.2 mol/L HCl. A high-performance liquid chromatography method with an ultraviolet detector (UV) was developed and validated. This method demonstrated superior sensitivity compared to existing methods, with a limit of detection (LOD) of 0.0237 μg/g, limit of quantification (LOQ) of 0.0829 μg/g, method limit of detection (MLOD) of 0.10 μg/g and method limit of quantitation (MLOQ) of 0.25 μg/g. The modified method exhibited excellent linearity for TMP in the range of 0.1–118.4 μg/mL, with a good correlation coefficient (R 2 > 0.999). The recovery rate of TMP in vinegar products ranged from 82.4 to 96.2%. Consequently, the proposed method exhibits substantial promise for systematic inquiry into TMP formation mechanisms and for ensuring consistent quality control during the production of premium-grade vinegars.
研究领域:
食品科学
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分析化学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 10
·e70136
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IF 1.7
Yiyao Zhang,Guangyun Zhang,Fen Yang,Zhikang Zou
Hemoglobin A 1c (HbA 1c ) plays a role in the diagnosis and assessment of glycemic control in patients with diabetes. However, few studies have focused on the preparation methods and analytical performance evaluation of different formulations of mobile-phase buffers for HbA 1c assays. In this study, mobile-phase buffers of new formulations were prepared for the measurement of HbA 1c . Following the Clinical and Laboratory Standards Institute (CLSI) guidelines, the analytical performance of newly developed mobile-phase buffers was evaluated. The CVs of the intra- and inter-assay precision were less than 0.94%, the RDs of accuracy were less than ± 3.00%, and the carryover was 0.00%. The measured HbA 1c values were linear from 4.50% to 16.80% (26.00–160.00 mmol/mol). A comparison of newly developed and commercial mobile-phase buffers revealed that the Pearson regression equation was Y = 0.9862 x + 0.0888 ( R 2 = 0.9990), and the Bland–Altman mean difference between the two mobile-phase buffers was −0.02833% (95% CI: −0.1853% to 0.1278%). The chromatography column had a lifetime of over 7000 tests. The reference interval was 4.30%–6.30% (23.00–45.00 mmol/mol). Stability was acceptable within 24 months. The newly developed mobile-phase buffers demonstrated good analytical performance (i.e., precision, linearity, accuracy, carryover, reference interval, the number of chromatography column runs, and stability).
研究领域:
临床化学
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糖尿病诊断
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分析方法验证
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色谱分析
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2024
·
IF 2.8
Peng Wang,Qiuliang Xu,Hua Zou,Ming Liu,Xiangjing Gao,Hong Ren,Junlin Wang,Yiyao Cao
Accurate, reliable, and sensitive methods for the determination of eight metabolites of p-chloronitrobenzene (p-CNB) were developed based on ultra-performance liquid chromatography − quadrupole − orbitrap high resolution mass spectrometry (UPLC-Q-Orbitrap HRMS). The free and conjugated forms of metabolites were determined before and after urine samples were hydrolyzed with acid. Subsequently, three solid phase extraction steps were used for concentration and purification. The calibration curves of the eight metabolites exhibited good linearity with an R 2 of >0.999, and the precision was good as well, with the coefficient of variations of intra-day and inter-day being lower than 7.0 % and 8.5 %, respectively. Analytical accuracy for all metabolites varied within ranges of 76.0–102.9 %, and the limit of detection and limit of quantification of all the metabolites varied within ranges of 0.2–7.7 μg/L and 0.6–25.6 μg/L in human urine, respectively. In addition, the application potential of the proposed methods were evaluated by applying them to the determination of metabolites in the urine of workers exposed to p-CNB, and these results showed that these methods were accurate, reliable, and sensitive, which makes them an excellent choice for detecting the metabolites of p-CNB in the urine of exposed workers.
研究领域:
分析化学
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环境健康
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职业健康
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2022
·Vol. 45
·期 13
·2161-2176
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IF 3.614
Yan-lin Zhao,Lin-lin Zhao,Yu-xin you,Xiao-xiao Zheng,Yan Du,Dao-quan Tang
We aim to establish a simple and easy high-performance liquid chromatography system coupled with an ultraviolet detector suitable for simultaneous determination of 24 antiepileptic drugs in human plasma. Optimized chromatographic separation was performed on a ZORBAX Eclipse Plus-C18 (4.6 × 150 mm 2 , 3.5 μm) column with acetonitrile and 5 mM potassium dihydrogen phosphate water solution as mobile phase. Note that, 24 antiepileptic drugs were divided into three groups and eluted with different gradient procedures, respectively. The column temperature was maintained at 35°C and the detection wavelength was set at 210 nm. Plasma was processed with ethyl acetate or acetonitrile. The calibration curves of 24 antiepileptic drugs demonstrated good linearity within the test range ( r > 0.996). The intra- and inter-batch precision and accuracy were all less than 15%, while extraction recoveries were in the range of 74.57–90.89% with the relative standard deviation values less than 15%. The validated methods have been successfully applied to determination of some antiepileptic drugs in rat or patient plasma. Those results indicated that the developed methods were simple and easy, and could be suitable for the determination of 24 antiepileptic drugs in plasma just by changing the gradient elution procedures of mobile phase.
研究领域:
分析化学
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药理学
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临床化学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2021
·Vol. 60
·期 2
·105-110
·
IF 1.618
Zhong ZhenHua,Chen YuPing,Xia HongYing,Chen ZhenZhen,Cheng QiZhen
A sensitive and selective gas chromatography–tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The linearity was established for the concentration range of 30–480 ng/mL (2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate) and 90–1440 ng/mL (chloromethane). The correlation coefficient of each PGIs was >0.995. The extraction recoveries ranged from 90.49 to 106.79% for the five PGIs. The quantitation limit, detection limit, accuracy, precision, repeatability and stability of the method demonstrated that the method was an adequate quality control tool for quantitation and identification of chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate at trace levels in drug substances and drug products.
研究领域:
药物分析
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分析化学
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药品质量控制
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产品关联
DOI
PubMed
高影响因子
ACS Applied Materials & Interfaces
·
2024
·
IF 8.3
Wanfang Feng,Yuyan Hu,Maoqing Wang,Li-Yan Liu
Enrichment and quantification of sugar phosphates (SPx) in biological samples were of great significance in biological medicine. In this work, a series of zirconium-based metal–organic frameworks (MOFs) with different degrees of defects, namely, HP-UiO-66-NH2-X, were synthesized using acetic acid as a modulator and were utilized as high-capacity adsorbents for the adsorption of SPx in biological samples. The results indicated that the addition of acetic acid altered the morphology of HP-UiO-66-NH2-X, with corresponding changes in pore size (3.99–9.28 nm) and specific surface area (894.44–1142.50 m2·g–1). HP-UiO-66-NH2-10 showed the outstanding performance by achieving complete adsorption of all four SPx using only 80 μg of the adsorbent. The excellent adsorption efficiency of HP-UiO-66-NH2-10 was also obtained with a wide pH range and short adsorption time (10 min). Adsorption experiments demonstrated that the adsorption process involved chemical adsorption and multilayer adsorption. By utilizing X-ray photoelectron spectroscopy and density functional theory to explain the adsorption mechanism, it was found that various interactions (including coordination, hydrogen bonding, and electrostatic interactions) collectively contributed to the exceptional adsorption capability of HP-UiO-66-NH2-10. Those results indicated that the defect strategy not only increased the specific surface area and pore size, providing additional adsorption sites, but also reduced the adsorption energy between HP-UiO-66-NH2-10 and SPx. Moreover, HP-UiO-66-NH2-10 showed a low limit of detection (0.001–0.01 ng·mL–1), high precision (<13.77%), and accuracy (80.10–111.83%) in serum, liver, and cells, good stability, high selectivity (SPx/glucose, 1:100 molar ratio), and high adsorption capacity (292 mg·g–1 for SPx). The practical detection of SPx from human serum was also verified, prefiguring the great potentials of defective zirconium-based MOFs for the enrichment and detection of SPx in the biological medicine.
研究领域:
分析化学
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材料科学
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生物医学工程
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生物化学
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产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2019
·Vol. 83
·期 1
·107-113
·
IF 1.552
Zhou Feng,Ren Xianghong,Du Siyan
Abstract Current methods for measurement of unsymmetrical dimethylhydrazine (UDMH) in wastewater suffer from a small detection range and complex pretreatment. In this study, ion chromatography (IC) with conductivity detection was used to directly analyze UDMH in wastewater, without any derivatization pretreatment, and the measurement range was as wide as 0.5–1000 μg·mL −1 . The effects of column temperature and sample pH on the detection were investigated. Furthermore, the chromatography conditions were optimized by combining the effects of different combinations of nitric acid, 2,6-pyridinedicarboxylic acid (PDCA), and methanesulfonic acid (MSA) on the analysis of mixed samples of UDMH and alkali metal ions. The linearity of the detected peak height ( H ) and peak area ( A ) versus UDMH concentration was studied at low, medium, and high concentrations. A good linear relationship was observed in the range of 0.5–1000 μg·mL −1 , especially for A , the relative standard deviation (RSD) and correlation coefficient ( R 2 ) of which were 0.077–1.653% and 0.9998–1.0000, respectively. In addition, the method showed good sensitivity with a limit of detection (LOD) of 0.05 μg·mL −1 and a limit of quantitation (LOQ) of 0.16 μg mL −1 . The precision and accuracy (expressed by recovery) were verified, where the RSD were less than 1.49% and 3.17%. Interference between hydrazines and alkali metal ions was discussed. Finally, actual UDMH samples were determined, confirming the applicability of the developed method for analyzing UDMH in wastewater during the degradation process. Graphic Abstract
研究领域:
环境化学
·
分析化学
·
废水处理
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DOI
高影响因子
危险品化学品经营许可证（带存储）