CHROMATOGRAPHIA
·
2022
·Vol. 85
·期 7
·589-603
·
IF 2.213
Zhong Hui,Zeng Qingli,Huang Zhiqin,Li Laisheng
Ferrocene is a stable metallocene complex with aromatic high-electron π-conjugated system and sandwich structures. We first prepared and characterized a novel ferrocenediamide bridged bis (β-cyclodextrin) chiral stationary phase (FeCDP) to explore its chiral separation function. Its HPLC performance was systematically evaluated by basic, acidic, amphoteric and neutral chiral probes, including triazoles, profens, flavanones, amino acids and β-blocker drugs in reversed-phase and polar organic modes, respectively. The results showed that FeCDP successfully resolved 44 kinds of tested analytes ( R s = 0.66–4.38), of which 36 were completely separated ( R s ≥ 1.5). The best resolutions of different types, such as hexaconazole, ketoprofen, 3'-hydroxyflavanone, phenylalanine and arotinolol on FeCDP were reached at 3.06, 1.90, 4.38, 1.89 and 2.12 in a short time, respectively. Especially, FeCDP could completely resolve imazalil ( R s = 1.97), ketoprofen ( R s = 1.90), dansylated arginine (Dns-Arg, R s = 1.50), pindolol ( R s = 1.42), bevantolol ( R s = 1.41), which were very difficult to be resolved on the conventional CDCSPs. However, under optimal condition, the ordinary CDCSP could only separate 19 analytes with low resolutions ( R s = 0.29–1.27). Compared with the reported similar stationary phases, the HPLC performance of FeCDP was also further improved. Based on the above comparison results, the satisfactory enantioselectivity of FeCDP may be mainly due to the fact that the “ pseudo -cavity” composed of two CDs and a ferrocene diamide, could provide cooperative inclusion for analytes. Meanwhile, the large π-conjugated ferrocenediamide bridging group could also provide hydrogen bonding, π–π stacking, dipole–dipole and hydrophobic interactions, which may promote the chiral recognition effect of FeCDP. Bridge CD-CSP was a versatile chiral separation material in drugs analysis. Graphical Abstract
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JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2022
·Vol. 61
·期 7
·625-636
·
IF 1.555
Zhong Hui,Zhang Tianci,Zeng Qingli,Li Laisheng
An azobenzenediamide bridged bis(β-cyclodextrin) chiral stationary phase (AZCDP) was prepared, and its high-performance liquid chromatography performance in reversed-phase and polar organic modes was evaluated by chiral probes, including triazoles, flavanones, amino acids and β-blockers. The results showed that AZCDP had strong chiral separation ability and the 40 chiral compounds were successfully resolved, of which 32 were completely separated (Rs ≥ 1.5) and the best enantioresolution was up to 3.93 within 20 min under a wide range of pH value and temperature. The separation ability of AZCDP with double cavities was significantly better than common CD-CSPs with single cavity, which was related to the synergistic inclusion effect. Compared with the previously reported stilbene (C=C)-bridged CSP, AZCDP with azobenzene (N=N)-bridged had a wider resolution range. For example, it could resolve myclobutanil, pindolol, carteolol, betaxolol, bevanolol and bitertanol, which could not be resolved before, and should be related to the fact that the flexible N=N was more compatible with the synergistic inclusion between cavities than the rigid C=C bridge group. The azobenzenediamide bridging group could also provide hydrogen bond, π–π and other sites, which was conducive to chiral separations.
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TALANTA
·
2021
·
IF 6.057
Tianhao Wu,Gongwei Sun,Mingying Ma,Xingyu Pan,Sichun Zhang,Xinrong Zhang
Developing rapid and reliable method for simultaneous hormones quantitation is of great significant because of important roles of hormones in metabolism. However, current methods are faced with problems of low throughput or complicated operation procedure to remove matrices from serum samples in routine clinical diagnosis. In the present work, a multilayer PS-MS method was developed for rapid and simple detection of hormones. In the strategy, multilayer filter paper acted as the Liquid Chromatography in LC-MS/MS for separation of hormones and biological matrices. Qualitative and quantitative analysis of three hormones, testosterone (T), androsterone (ADT) and androstenedione (4-AD) were realized through MS/MS spectra. The method exhibited linearity in the range of 0.02–2 μg/L and the results of recovery and repeatability were satisfactory for standard samples and spiked serum. The time-cost of a whole detection process was less than 3 min. The established multilayer PS-MS realized rapid, simple and reliable quantitative analysis of various hormones and provided broad prospect for clinical analysis of small molecules in different biological samples. Moreover, it provides a novel MS approach with high through-put and free HPLC, meeting the requirements of point-of-care testing (POCT).
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高影响因子
ANALYTICAL SCIENCES
·
2021
·Vol. 37
·期 8
·1095-1103
·
IF 2.081
Tianci ZHANG,Yazhou SHUANG,Hui ZHONG,Liang LI,Laisheng LI
A new β-cyclodextrin-bonded chiral stationary phase (TCDP) with a thiocarbamated benzamide spacer was prepared and evaluated on HPLC by separating a series of chiral pesticides and drugs. TCDP resolved all 24 analytes (11 triazoles, 8 flavanones and 5 β-blockers), and 18 of them were completely separated. The enantioresolution ranges were 1.45 – 3.33 for triazoles, 0.35 – 2.45 for flavanones and 1.26 – 1.58 for β-blockers. Among them the best resolution of tebuconazole was up to 3.33 within 13 min. Bitertanol (two chiral centers) and triticonazole with cis/trans isomers were separated into four peaks, respectively. TCDP could also completely resolve myclobutanil (Rs = 1.68), which was difficult to be separated on other CD-CSPs. Common CDSP only resolved a few analytes. The results showed that the thiocarbamated benzamide spacer of TCDP may provide a synergistic effect of hydrogen bonding and coordination. The spacer deserved full utilization, by which may avoid troublesome derivatization at low cost.
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MICROCHIMICA ACTA
·
2021
·Vol. 188
·期 9
·1-10
·
IF 5.833
Guo Ping,Yuan Bao-Yan,Yu Yun-Yan,Zhang Jun-Hui,Wang Bang-Jin,Xie Sheng-Ming,Yuan Li-Ming
The fascinating framework structures and unique properties of chiral covalent organic frameworks (COFs) make them promising candidates as novel separation medium for high-performance liquid chromatography (HPLC). However, the irregular morphology, inhomogeneous particle size, and low density of conventional COF particles will lead to a low column efficiency, undesirable chromatographic peak shape, and high column backpressure of such COF-packed columns. In this work, a chiral COF CTpBD was synthesized by the Schiff base reaction between benzidine (BD) and chiral organic monomer CTp obtained through the reaction of 1,3,5-triformylphoroglucinol (Tp) and (+)-diacetyl-L-tartaric anhydride ((+)-Ac-L-Ta). The chiral COF CTpBD was immobilized on the surface of amino functionalized silica (SiO 2 -NH 2 ) by an in situ growth approach to prepare the chiral COF core-shell microsphere composite CTpBD@SiO 2 , which was used as a novel chiral stationary phase (CSP) for HPLC enantioseparation. Various kinds of racemates were separated on the CTpBD@SiO 2 -packed column with a low column backpressure (8–11 bar). Some effects such as the analyte mass and column temperature on the HPLC enantioseparation have been studied in detail. The fabricated CTpBD@SiO 2 -packed column exhibited high column efficiency (e.g., 16,800 plates m −1 for atenolol), high enantioselectivity, and good reproducibility toward various racemates. The highest resolution value, retention factor, and separation factor reach to 2.11, 2.85, and 3.73, respectively. The relative standard deviations (RSD) of peak area, peak height, half-peak width, and retention time of atenolol were all below 3.0%. Graphical abstract
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高影响因子
NEW JOURNAL OF CHEMISTRY
·
2021
·Vol. 45
·期 15
·6856-6864
·
IF 3.591
Hao Li,Xiaomei Song,Pengfei Li,Wen Li,Ting Wang,Liting Qin,Juying Zhou,Fuhou Lei
Rosin-based polymer microspheres (RPMs) as stationary phases in HPLC were prepared using methyl acrylic acid as the functional monomer, ethylene glycol maleic rosinate acrylate as the cross-linker, and a carboxylic group as the major functional group. The obtained RPMs were characterized by different analytical techniques. The results indicated that the RPMs have a regular spherical shape with porous surfaces, an average particle size of 5.5 μm, a surface area of 96.73 m2 g−1, and an average pore size of 11.68 nm. Moreover, the RPMs displayed good thermal stability. Theophylline, caffeine, tetrahydropalmatine, and berberine hydrochloride were used as probes to study the separation properties of alkaloids and their analogs on an RPM chromatographic column. Theophylline/caffeine and tetrahydropalmatine/berberine hydrochloride were separated by a rosin-based chromatographic column under optimum chromatographic conditions, and their resolution factors were 5.29 and 3.72, respectively. Furthermore, the chromatographic thermodynamics and separation mechanism were also studied. Thermodynamic data obtained by van’t Hoff plots showed that their separation on the RPM chromatographic column was an enthalpy-driven exothermic process. Microcalorimetry and zeta potential were employed to investigate the separation mechanism of the binding of alkaloids to the rosin-based polymer surface. The RPM and theophylline (or caffeine) interact through hydrogen bonding interactions, whereas the interactions between the RPM and tetrahydropalmatine (or berberine hydrochloride) arose from hydrogen bonding and electrostatic attraction.
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2021
·
IF 1.312
Xinyu Wang,Xiaohan Wei,Qingfa Tang,Wei Zhong Huang,Yunxia Teng,Zhizhong Liao,XiaoMei Tan,Xin Mao,Xinyu Wang and Xiaohan Wei are common first authors
Fici Microcarpae Folium, the leaves of Ficus microcarpa, is commonly used for the treatment of influenza, chronic bronchitis, and tonsillitis in Traditional Chinese Medicine (TCM). Ficus microcarpa is mainly distributed in Guangdong and Guangxi provinces. The composition of herbal medicines can be easily affected by geographical regions, the quality control of FMF is essential. In this study, the high-performance liquid chromatography (HPLC) coupled with diode array detection (DAD) was developed to obtain a chromatographic fingerprint of Fici Microcarpae Folium from different geographical regions. Meanwhile, the contents of eight compounds of Fici Microcarpae Folium were determined. Principal component analysis (PCA), hierarchical cluster analysis (HCA), and orthogonal partial least squares discrimination analysis (OPLS-DA) were employed to evaluate the HPLC fingerprint. The results showed that the main compositions of Fici Microcarpae Folium from different geographical origins had no difference. The content of the main compositions was different, from which the peak 8, 15, 12, 11, 16, 3, and 21 were the main components that contribute to the difference. Isovitexin, vitexin, and isoorientin were the main components reflecting the quality of Fici Microcarpae Folium. This research could contribute to the quality control of Fici Microcarpae Folium.
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CHROMATOGRAPHIA
·
2019
·Vol. 83
·期 2
·205-217
·
IF 1.552
Li Li,Chen Naijiang,Gu Puzhong,Li Honglei,Li Mengqing,Zhang Ziyue,Chen Ruiling,Zhang Ming
Abstract Compound amino acid injection-18 AA (CAAI-18 AA) is widely applied in medical care as a part of total parenteral nutrition systems. Thus, suitable quality control of CAAI-18 AA is of crucial importance for safety of the patients. Tryptophan (TRP) is one of the main components in CAAI-18 AA and may be degraded to 5-hydroxy-tryptophan (5-HTP), 5-hydroxytryptamine (5-HT), kynurenine (KYN) and indole (IN) under certain conditions, such as oxidation environments, ultraviolet light radiation and nonsterile conditions. The existence of these harmful impurities seriously affects the quality of CAAI-18 AA. Here, a simple HPLC approach with a PDA detector was developed and validated for simultaneous determination of the concentrations of 5-HTP, 5-HT, KYN and IN impurities in CAAI-18 AA. Separation of these four impurities in CAAI-18 AA was achieved under a gradient condition using acetonitrile and 10 mM phosphate buffer (containing 10 mM sodium 1-octanesulfonate, pH adjusted to 1.8 with phosphoric acid). To detect the four analytes with high sensitivity, multi-wavelength detection at 257, 270 and 276 nm was carried out during the separation. The method was validated in accordance with ICH guidelines and the results were compared to that obtained by UHPLC–MS/MS, showing that the two approaches did not provide significantly different results. Our results reveal that the simple and less expensive HPLC method holds great potential for quantitation of the four impurities in CAAI-18 AA. Graphic Abstract
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JOURNAL OF COLLOID AND INTERFACE SCIENCE
·
2015
·
IF 3.368
Ling Zhu,Guanhong Xu,Fangdi Wei,Jing Yang,Qin Hu
A novel molecularly imprinted stir bar (MIP-SB) was developed with melamine (MA) as the template molecule in this study. The sorptive capacity of MIP-SB was nearly three times over that of non-imprinted stir bar (NIP-SB). The MIP-SB presented much better selectivity than NIP-SB when used to absorb MA and its analogues. An analytical method to determine MA in powdered milk was established by combining MIP-SB sorptive extraction with HPLC. The liner range was 0.0631–12.6 ng/mL with good correlation coefficient of 0.9983, and the limit of detection was 0.0127 ng/mL based on three times ratio of signal to noise. This method was successfully applied to the determination of MA in powdered milk with satisfactory results. The method built is simple and suitable for the determination of MA in milk products which is of great significance for quality control of milk products.
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GLYCOCONJUGATE JOURNAL
·
2017
·Vol. 34
·期 5
·625-632
·
IF 2.186
Song Shuang,Yu Qi,Zhang Bao,Ai Chunqing,Sun Yujiao,Fu Yinghuan,Zhao Meiyu,Wen Chengrong
Fish intestines and livers are usually considered as delicious and nutritious food in China. Acidic polysaccharides are important nutrients in these food of animal origin, but there is currently little information regarding their quantitative distributions. The present study demonstrated a method to quantify acidic polysaccharides simultaneously by analyzing their disaccharides produced from the acid hydrolysis using high-performance liquid chromatography (HPLC) coupled with triple quadrupole mass spectrometry. The recoveries for these acidic polysaccharides were all 97%–115% with relative standard deviation of 3.0%–9.0%. All of the acidic polysaccharides had good linearities. Then this method was applied to determine the composition of acidic polysaccharides in 5 edible fish livers and intestines. Besides well-known glycosaminoglycans (GAGs) including hyaluronic acid (HA), Chondroitin sulfate (CS), dermatan sulfate (DS) and heparin (HP), 4 novel acidic polysaccharides including 2 GAGs and 2 non-GAGs comprised of hexose-hexuronic acid repeating units were also found. CS and HP were the major acidic polysaccharides components in fish intestines and livers, respectively. The absolute amounts of acidic polysaccharides differed greatly in these fish tissues, but their proportions showed similarity in the same type of tissues. The present study demonstrated an effective method for acidic polysaccharides quantification, and revealed acidic polysaccharides compositions of edible fish livers and intestines.
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ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2016
·Vol. 23
·期 19
·19409-19416
·
IF 2.76
Peng Guilong,He Qiang,Lu Ying,Mmereki Daniel,Zhong Zhihui
A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid–liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2–500 ng/g, with the correlation coefficients ( r ) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12–0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25–6.26 % ( n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Yang Yang,Ying Lian,Ping Zhong,Dandan Wang,Bin Di,Bo Li
Ten related substances in coenzyme A (CoA) were detected using a newly developed gradient reverse phase high performance liquid chromatographic (HPLC) method. A highly specific and efficient LC–MS/MS method was developed to characterize process-related substances and the major degradation products, and three unknown related substances were further synthesized and characterized by H-NMR and C-NMR spectroscopy. Synthesized samples of the related substances were used for quantitative analysis by HPLC. The method was validated according to ICH guidelines with respect to specificity, precision, accuracy and linearity. The forced degradation studies included acidic, alkaline, oxidative, photolytic and thermal stress conditions. Furthermore, we depicted and speculated the probable mechanism of formation of related substances and the plausible fragmentation mechanism showed that all the related substances came from the manufacturing process. Characterization, synthesis and quantitative analysis of related substances were discussed in detail, and were critical for quality control, manufacturing process optimization and CoA monitoring, all of which were important to ensure the security of CoA.
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危险品化学品经营许可证（带存储）