REVIEWS IN ANALYTICAL CHEMISTRY
·
2024
·Vol. 43
·期 1
·
IF 3.6
Xiaoxi Si,Yu Tian,Shufang Xu,Chunbo Liu,Zhenjie Li,Ji Yang,Ying Guan,Yangzhou Xie,Xiaoqing Shi,Zhigang Xu,Zhihua Liu
Alkaloid enantiomers have different physiological and pharmacological effects, and different chiral compositions have a large impact on cigarette sensory and use safety. Studying the effects of different configurations of alkaloid enantiomers on cigarette sensory is important for the development of tobacco products, but the chiral separation of alkaloid enantiomers has become the core problem. Here, the application of a C18 column coupled with a polysaccharide-based chiral column to separate and detect four pairs of alkaloid enantiomers in tobacco and cigarette smoke of different brands was investigated. Results showed that the tandem technology of the two columns enabled the baseline separation of four pairs of alkaloid enantiomers. The resolution of enantiomers of alkaloids in different tobacco samples differed in content and ratio, showing different chiral distribution characteristics. According to the different distribution characteristics of alkaloid enantiomers, tobacco samples of different brands can be distinguished and real cigarettes can be identified.
研究领域:
分析化学
·
烟草科学
·
药物化学
✓ 已验证
产品关联
DOI
高影响因子
Systems Microbiology and Biomanufacturing
·
2025
·
IF 2.9
Shi Yu,Li Huifan,Lu Yuqi,Chen Ming,Yang Hua,Fu Dongmei
A simple and robust reversed-phase high performance liquid chromatography procedure was developed with only an aqueous H 3 PO 4 solution (pH 2.1) as the mobile phase for the simultaneous determination of nine organic acids (oxalic, formic, malic, lactic, acetic, citric, succinic, fumaric, and gallic acids) in beer based on a polar-copolymerized 3-chloropropyl C18 column. The proposed method was validated according to linearity, limits of detection, accuracy, precision, repeatability, and reproducibility. Quantifications of the nine organic acids in 12 commercial Chinese beer samples from five different brands were conducted only after degassing and filtration of the samples. In all beer samples, the most abundant organic acid was succinic acid; its concentration was in the range of 907.99–3557.22 mg/L. This was followed by malic acid (170.39–936.78 mg/L). Principal component analysis was used to compare the different brand of beers according to organic acid concentration, and results may provide a reference for the evaluation of beer quality and taste.
研究领域:
分析化学
·
食品科学
·
色谱技术
✓ 已验证
产品关联
DOI
高影响因子
TALANTA
·
2015
·
IF 3.545
Ting Tan,Mingliang Zhang,Yiqun Wan,Hongdeng Qiu
Deep eutectic solvents (DESs) were used as novel mobile phase additives to improve chromatographic separation of four quaternary alkaloids including coptisine chloride, sanguinarine , berberine chloride and chelerythrine on a C 18 column. DESs as a new class of ionic liquids are renewably sourced, environmentally benign, low cost and easy to prepare. Seven DESs were obtained by mixing different hydrogen acceptors and hydrogen-bond donors. The effects of organic solvents, the concentration of DESs, the types of DESs and the pH values of the buffer solution on the separation of the analytes were investigated. The composition of acetonitrile and 1.0% deep eutectic solvents aqueous solution (pH 3.3, adjusted with hydrochloric acid) in a 32:68 (v/v) ratio was used as optimized mobile phase, with which four quaternary alkaloids were well separated. When a small amount of DESs was added in the mobile phase for the separation of alkaloids on the C 18 column, noticeable improvements were distinctly observed such as decreasing peak tailing and improving resolution. The separation mechanism mediated by DESs as mobile phase additives can be attributed to combined effect of both hydrogen acceptors and hydrogen-bond donors. For example, choline chloride can effectively cover the residual silanols on silica surface and ethylene glycol can reduce the retention time of analytes. The proposed method has been applied to determine BerbC in Lanqin Chinese herbal oral solution and BerbC tablet. Utilization of DESs in mobile phase can efficiently improve separation and selectivity of analytes from complex samples.
研究领域:
分析化学
·
药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2020
·Vol. 412
·期 6
·1365-1374
·
IF 3.637
Luo Qiurong,Ren Xiujun,Wei Siping,Zheng Yunchao,Gao Die,Fu Qifeng,Xia Zhining,Wang Lujun
Molybdenum disulfide quantum dots (MoS 2 QDs) were chosen as a functional two-dimensional material to improve the separation performance of a traditional C18 column. In this work, MoS 2 QDs were synthesized by the combination of sonication and solvothermal treatment of bulk MoS 2 . The prepared MoS 2 QDs were characterized by transmission electron microscope (TEM), Zeta potential measurement, UV-visible absorption and fluorescence spectroscopy. Then, a novel MoS 2 QDs embedded C18 (Sil-MoS 2 -C18) stationary phase was prepared for performing mixed-mode liquid chromatography. The results of elemental analysis (EA), thermogravimetric analysis (TGA), Fourier transform infrared spectrometry (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM) and Brunauer-Emmett-Teller (BET) measurements indicated the stationary phase was prepared successfully. Five types of compounds including alkylbenzenes, polycyclic aromatic hydrocarbons (PAHs), nucleosides and nucleobases, anilines and flavonoids were utilized to evaluate reversed phase, weak cation exchange and hydrophilic interaction of the new column. To a certain extent, the column could achieve separation for different properties of samples on one column, with less organic solvent and shorter time than conventional alkyl and amino columns. Furthermore, the mechanism for separation was studied by investigating effects of mobile phase composition and pH on retentions. In summary, the Sil-MoS 2 -C18 stationary phase was deemed able to serve the performance of various types of phases, which revealed the prepared mixed-mode column could be potentially applied for the analysis of complex samples.
Graphical abstract
研究领域:
分析化学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2023
·Vol. 15
·期 7
·884-895
·
IF 3.1
Xin Wang,Xiaoqi Sun,Yueying Jin,Shengyu Cheng,Yu Han,Minghui Zhang,Lingli Zhang,Xi-Ling Li,Chun-Yan Xu,Jun Zhe Min
This study reports a novel fluorescent chiral derivatization reagent, 4-(N,N-dmethylaminosulfonyl)-2,1,3-benzoxadiazole-(2-succinimidoxy)-trans-2-methyl-L-proline (DBD-S-M-Pro), with a benzoxadiazole structure containing an N-hydroxysuccinimide activation group. DBD-S-M-Pro targets chiral amino-functional compounds under alkaline conditions without a condensation agent. Gradient elution was performed on a BEH C18 (100 × 2.1 mm, 1.7 μm) column with a mobile phase of 0.05% formic acid (FA) in 10 mM ammonium acetate (CH3COONH4) and 0.1% FA in acetonitrile or methanol. The efficiency of the chiral resolution was evaluated under excitation and emission wavelengths of 450 nm and 560 nm, respectively. The 19 chiral amino acids were separated in the range of 1.45–14.84. The resolutions of almost all DL-amino acids exceeded 1.5; the exceptions were serine (Ser) and lysine (Lys), with resolutions of 1.45 and 1.46, respectively. In addition, a new approach was devised for the simultaneous analysis of four chiral amino acids (DL-Glu, DL-Ala, DL-Val, and DL-Phe) in human hair. These amino acids were analyzed in the range of 12.5–400 pmol, with R2 ≥ 0.9990, limits of detection (S/N = 3) of 4–10 pmol, and intraday and interday precisions of 0.57–6.23%. The average spikes in the hair recoveries were 89.76–111.54%, and the matrix effects were 92.47–102.40%. Next, the contents of free chiral amino acids in the hair samples of 10 healthy volunteers (five males and five females) were analyzed with this method, and the differences were compared. The developed DBD-S-M-Pro provides a novel strategy for the sensitive determination of free chiral amino acids in living organisms.
研究领域:
分析化学
·
生物化学
·
药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2012
·Vol. 50
·期 7
·620-624
·
IF 0.884
Xie Kaizhou,Jia Longfei,Xu Dong,Guo Huisheng,Xie Xing,Huang Yuping,Chen Xuesen,Bao Wenbin,Dai Guojun,Wang Jinyu
A sensitive and robust method is presented for the simultaneous determination of amoxicillin (AMO) and ampicillin (AMP) in eggs by reversed-phase high-performance liquid chromatography with fluorescence detection (RP-HPLC–FLD). This method used a simple liquid–liquid extraction of the samples with acetonitrile and dichloromethane as precipitation of proteins and extraction solvent. AMO and AMP reacted with salicylaldehyde to form fluorescent derivatives, which were then analyzed with RP-HPLC–FLD. Separation was carried out on an Athena C18 column with a mobile phase consisting of 0.01M potassium dihydrogen phosphate, adjusted to pH 5.5 by 2M potassium hydroxide and acetonitrile. The detector response was linear over the tested concentration range from 5.0 to 800 ng/mL for AMO and AMP. The recovery values ranged from 78.4 to 88.7% for AMO and from 77.6 to 82.0% for AMP. The limits of detection were 1.2 for AMO and 0.4 µg/kg for AMP. The limits of quantification were 3.9 for AMO and 1.5 µg/kg for AMP. The corresponding intra-day and inter-day variation (relative standard deviation) were found to be less than 9.6 and 14.8%, respectively.
研究领域:
分析化学
·
食品科学
·
药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Heliyon
·
2023
·
IF 4
Hengyi Yu,Dongyan Li,Dong Xiang,Xiping Li,Lu Liu,Dong Liu,Xuepeng Gong
A rapid, specific and accurate high-performance liquid chromatography with tunable ultraviolet detection method was developed to simultaneously determine azathioprine metabolites, 6-thioguanine nucleotides (6-TGN) and 6-methyl mercaptopurine riboside (6-MMPr) in human red blood cells. Erythrocyte lysate sample was precipitated by perchloric acid under the protection of dithiothreitol, with 6-TGN and 6-MMPr being acid hydrolyzed to produce 6-thioguanine (6-TG) and 6-methymercaptopurine (6-MMP). A Waters Cortecs C 18 column (2.1 × 150 mm, 2.7 μm) was used for chromatographic separation with a water (containing 0.01 mol/L ammonium acetate and 0.2% acetic acid)/methanol linear gradient at a flow rate of 0.45 mL/min in a 5.5 min. UV detection wavelengths were 340 nm for 6-TG, 303 nm for 6-MMP and the IS (5-bromouracil). The calibration curves fitted a least squares model (weighed 1/ x 2 ) from 0.15 to 15 μmol/L for 6-TG ( r 2 = 0.9999) and from 1 to 100 μmol/L for 6-MMP ( r 2 = 0.9998). This method was validated according to the FDA bioanalytical method validation guidance and ICH M10 bioanalytical method validation and study sample analysis guidance for industry, and successfully utilized in ten IBD patients receiving azathioprine therapy.
研究领域:
药理学
·
分析化学
·
临床化学
✓ 已验证
DOI
PubMed
高影响因子
RSC Advances
·
2024
·Vol. 14
·期 46
·34261-34269
·
IF 3.9
Min Xie,Jun Xu,Dan Fei,Ye-Lan Guang,Yao-Min Zhou,Fan Li,Li-Zhen Hu
An improved QuEChERS method combined with Multi-Plug Filtration Cleanup (m-PFC) clean-up procedure was developed for the simultaneous determination of 16 different sulfonamides in forage grasses using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The forage grass sample was extracted with 0.1 mol L−1 Na2EDTA-Mcllvaine buffer and acetonitrile solution, purified by the Navo U-QuE column tube, separated by Agilent ZORBAX Eclipse Plus C18 column, and analyzed by MRM (multiple reaction monitoring) mode and the internal standard method was utilized for quantification. The 16 different sulfonamides display good linearity within the range of 0.5–50 μg L−1 (R2 > 0.9967), the limit of detection was 0.02–0.5 μg kg−1, and the limit of quantification was 0.05–1.0 μg kg−1. Under the additive amounts of 1, 2, and 10 μg kg−1, the recoveries were in the range of 72.3–116.9%, and the relative standard deviation was between 1.4% and 10.3%. The presented method showed the advantages of simple operation, excellent selectivity and high sensitivity. It was well-suited for both qualitative and quantitative analyses of sulfonamides in forage grass. Overall, this method provided a scientific basis for risk assessment, enforcement of quality and safety standards, and detection of sulfonamide residues in forage grass for import and export.
研究领域:
分析化学
·
兽医学
·
食品安全
·
药物分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Zhefei Hu,Yanhao Jiang,Panpan Cao,Yanjuan Liu,Yuefei Zhang,Wei Chen,Sheng Tang
In this work, 2-undecylimidazole (UI) and propyl methacrylate (PMA) dual-functionalized silica gel was prepared and applied as a mixed-mode chromatographic stationary phase. Successful preparation of this stationary phase (SiO 2 -UI-PMA) was proved through a range of characterization techniques. The chromatographic performance of the obtained SiO 2 -UI-PMA was investigated for the separation of environmental endocrine disruptors (phthalates, steroid hormones, bisphenols and alkylphenols), sulfonamides and food-borne stimulants in reversed-phase chromatography, as well as for the separation of inorganic anions in anion-exchange chromatography. The effect of column temperature, acetonitrile content, salt concentration and mobile phase pH on retention was studied to explore the separation mechanism, and the results indicated that this stationary phase provided multiple interactions with analytes. Compared with the commercial C18 column, the SiO 2 -UI-PMA demonstrated more preferable separation ability under the mobile phase conditions with a low content of acetonitrile, thereby acting as a good alternative candidate for the conventional reversed-phase stationary phase in chromatographic analysis. Furthermore, the SiO 2 -UI-PMA stationary phase exhibited high column efficiency (45 860 plates m −1 for progesterone) even though it was prepared from the non-serviceable silica based chromatographic packing materials.
研究领域:
分析化学
·
环境科学
·
材料科学
✓ 已验证
产品关联
DOI
高影响因子
危险品化学品经营许可证（带存储）