MICROCHIMICA ACTA
·
2023
·Vol. 190
·期 6
·1-9
·
IF 5.7
Liu Cheng,Guo Ping,Lu Yan-Rui,Zhu Yu-Lan,Ran Xiao-Yan,Wang Bang-Jin,Zhang Jun-Hui,Xie Sheng-Ming,Yuan Li-Ming
The manufacturing of chiral covalent triazine framework core-shell microspheres CC-MP CCTF@SiO 2 composite is reported as stationary phase for HPLC enantioseparation. The CC-MP CCTF@SiO 2 core-shell microspheres were prepared by immobilizing chiral COF CC-MP CCTF constructed using cyanuric chloride and (S)-2-methylpiperazine on the surface of activated SiO 2 through an in-situ growth approach. Various racemates as analytes were separated on the CC-MP CCTF@SiO 2 -packed column. The experimental results indicate that 19 pairs of enantiomers were well separated on the CC-MP CCTF@SiO 2 -packed column, including alcohols, phenols, amines, ketones, and organic acids. Among them, there are 17 pairs of enantiomers that can achieve baseline separation with good peak shapes. Their resolution values on this chiral column are between 0.4 and 5.61. The influences of analyte mass, column temperature, and composition of the mobile phase on the resolution of enantiomers were studied. In addition, the chiral resolution ability of CC-MP CCTF@SiO 2 -packed column was compared with the commercial chiral chromatographic columns (Chiralpak AD-H and Chiralcel OD-H columns) and some CCOF@SiO 2 chiral columns (β-CD-COF@SiO 2 , CTpBD@SiO 2 , and MDI-β-CD-modified COF@SiO 2 ). The CC-MP CCTF@SiO 2 -packed column exhibited some unique advantages and can complement these chiral columns in chiral separations. The research results show that the CC-MP CCTF@SiO 2 chiral column offered high column efficiency (e.g., 17680 plates m −1 for ethyl mandelate), low column backpressure (5–9 bar), high enantioselectivity, and excellent chiral resolution ability for HPLC enantioseparation with good stability and reproducibility. The relative standard deviations (RSD) ( n = 5) of the retention time, and peak areas by repeated separation of ethyl mandelate are 0.23% and 0.67%, respectively. It demonstrates that the CC-MP CCTF@SiO 2 core-shell microsphere composite has great potential in enantiomeric separation by HPLC. Graphical abstract
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JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2023
·
IF 3.4
Wanbing Rao,Lijun Li,Chenxia Zhang,Jinfu Zheng,Xiaomei Fan,Baolei Luan,Jiaxiang Sun,Meiyan Qiu,Shuming Wu,Yanhua Li,Zhongqing Wang
A simple and stability-indicating reverse phase high-performance liquid chromatographic (RP-HPLC) method for the determination of rivaroxaban (RIX) and its related substances was developed. Fifteen impurities of RIX, including three unreported isomers, were identified, synthesized, purified, and confirmed using MS, 1 H NMR, 13 C NMR, and HSQC spectral methods. This new method offered baseline separation for all monitored impurities, and was fast and reliable when compared to the European Pharmacopoeia method. Optimum separation for RIX and its related impurities was achieved on an octyldecyl silica column (YMC Core C18, 4.6 ×100 mm, 2.7 µm) by using a gradient HPLC method in 38 min. The final method was validated with respect to precision, LOD and LOQ, linearity, accuracy, and robustness. This developed method was suitable for routine quality control and drug analysis of RIX active substance.
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Natural Product Communications
·
2023
·
IF 1.8
Wenjia Li,Qinggui Lei,Wenqing Li,Guoying Tan,Xingzhong Liu,Zhengming Qian
A high-performance liquid chromatography (HPLC) method for the determination of 4 nucleosides by one reference compound in Chinese cordyceps was developed. The sample of Chinese cordyceps was prepared by ultrasonic extraction with a 0.5% phosphoric acid aqueous solution. The separation of the sample was performed on a CORTECS T3 column (100 mm × 4.6 mm, 2.7 μm) by gradient elution with acetonitrile and water at a flow rate of 1.0 mL/min. The wavelengths were set as 258 nm (0-5 min), 252 nm (5-9.1 min), 258 nm (9.1-10.5 min), 249 nm (10.5-20 min) at which 4 nucleosides exhibited identical ultraviolet absorption. The accuracy, precision, reproducibility, and stability tests of the HPLC method were carried out, and the results indicated that the established HPLC method was suitable for the quantitative analysis of 4 nucleosides in Chinese cordyceps. This approach was compared to the traditional external standard method with 4 nucleoside reference compounds and the relative standard errors of the content determination results by the 2 methods were less than 3.5%. The HPLC method developed for quantitative measurement of 4 nucleosides in Chinese cordyceps is simple, lower cost, and time-saving, which provides a methodology alternative for quality control of Chinese cordyceps.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 2
·1-8
·
IF 5.479
Ding Hui,Wang Rongyu,Liu Wei,Cheng Supan,Ji Wenhua,Zheng Zhenjia,Wang Xiao
The authors describe a new spherical metal-organic coordination polymer (MOCP) for use as an adsorbent in solid-phase microextraction (SPME). By applying the ions Co(II), Fe(II), Cu(II), and Zn(II) in these polymers, MOCP with different morphology were obtained. The respective coatings for SPME display different extraction efficiency towards neonicotinoid insecticides (neo-nics). The Co(II)@MOCP coating displays an improved extraction capability for neo-nics when compared to the four commercially available coatings studied. Following extraction with the Co(II)@MOCP-coated fiber, the neo-nics were eluted using 1 mL of trifluoroacetic acid/acetonitrile solution and quantified by high performance liquid chromatography. The method, when applied to spiked honey samples, has good linearity (0.5–600 μg kg −1 ) and a low limit of detection (0.05–0.15 μg kg −1 ). The precision ( n = 6) for a single fiber was in the range of 3.6–8.3%. The reproducibility (for n = 5) from fiber-to-fiber ranges between 5.4 and 8.8%. The Co(II)@MOCP-coated fiber can be reused more than 80 times without any apparent reduction in its performance. In addition, the relative recoveries from spiked honey samples are very good (91.5%–103.5%).
A spherical metal-organic coordination polymer (MOCP) was synthesized under the regulation of Co(II) and used for the solid-phase microextraction (SPME) of neonicotinoid insecticides found in honey.
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MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Lanyun Fang,Yumei Zhang,Beibei Lu,Li Wang,Xunping Yao,Ting Ge
The present paper proposed an analytical method for speciation analysis of inorganic antimony in inhalable particulate matter, PM2.5, using high performance liquid chromatography coupling with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A new extraction method consisted of reducing extraction and oxidizing extraction using EDTA as the key component in the extractant has obtained better extraction yield and preserves stability of both species during the extraction process. Stability of Sb species in EDTA-saturated nitric or tartric acid solution and in aqueous solution were carefully investigated. Using the optimized conditions, the method allows for the determination of Sb(III) and Sb(V) in PM2.5 samples with limits of 0.10 and 0.06 ng m −3 , respectively. The precision, expressed as relative standard deviation (RSD), was always lower than 8.5% and 6.6% for Sb(III) and Sb(V), respectively. The spiked recovery rates of Sb species at three different concentration levels were in the range of 90.0–110.0%. The extraction yield of the sequential extraction process confirmed by analysis of a certified reference material of urban particulate matter, NIST1648a, furnished by National Institute of Standards and Technology was 60%. This method was applied to determine Sb(III) and Sb(V) in PM2.5 samples collected in urban area in Ningbo City, China. The results showed that both Sb(V) and Sb(III) were found in most of the samples analyzed, Sb(V) being the main one, which represents 69–87% of the total Sb extracted in the considered samples, whereas Sb(III) represents the remaining 13–31%.
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MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 6
·1-10
·
IF 5.479
Liu Zikai,Lin Xiwen,Liu Xinya,Li Jing,Zhou Wenfeng,Gao Haixiang,Zhang Sanbing,Lu Runhua
A magnetic sorbent was fabricated by covalently grafting hyperbranched polyamidoamine onto the surface of Fe 3 O 4 nanoparticles. The sorbent was used in the magnetic solid-phase extraction (MSPE) of benzoylurea insecticides (BUs) from environmental water samples. It is perceived that hydrogen bonding interactions and hydrophobic interactions are the main mechanisms for the adsorption of BUs. The sorbent was characterized by scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy, elemental analysis, Brunauer-Emmett-Teller measurement, X-ray photoelectron spectroscopy, vibrating sample magnetometry and X-ray diffraction. Various experimental parameters affecting the MSPE were optimized. Following elution with acetonitrile, the BUs were quantified by HPLC with diode array detection. The method based has a wide linear response range (2.5–500.0 ng mL −1 ), satisfactory coefficient of determination (0.9922–0.9976), high enrichment factors (62.8–74.4), acceptable limits of quantitation (2.5 ng mL −1 ) and low limits of detection (0.39–0.72 ng mL −1 ). The intra-day precision at concentration levels of 5.0, 50.0 and 250.0 ng mL −1 ranged from 2.3–6.4% and the inter-day precision was between 1.0 and 5.5%. The sorbent can be re-used at least 15 times. It was applied to the extraction of BUs from genuine water samples where it showed satisfactory relative recoveries (75.1–111.4%) and precision (1.0–9.1%).
Schematic presentation of magnetic nanoparticles modified with hyperbranched polyamidoamine and their application for extraction of benzoylurea insecticides.
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FOOD CHEMISTRY
·
2018
·
IF 4.946
Si-Jin Liu,Juan-Juan Xu,Chang-Lu Ma,Chun-Feng Guo
The six biogenic amines in sausage and cheese were analyzed by HPLC with UV detection after off-line derivatization with dansyl chloride, 9-fluorenylmethoxycarbonyl chloride, benzoyl chloride and dabsyl chloride, respectively. The results showed that both the off-line 9-fluorenylmethoxycarbonyl and dabsyl derivatization were not suitable for HPLC analysis of biogenic amines when batch injection was used because the derivatives were instable, whereas both the off-line dansyl and benzoyl derivatization were suitable for HPLC analysis of biogenic amines when batch injection was used, but the latter needed to maintain the derivatives at 4 °C to ensure that benzoylated tyramine was not degraded when waiting for the analysis. The off-line dansyl derivatization had an obvious advantage in the analysis of biogenic amines in sausage and cheese samples by HPLC combined with batch injection because the method has a wider linear range and higher sensitivity, accuracy, precision and stability of the derivatives.
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TALANTA
·
2018
·
IF 4.244
Xiao Sun,Jing Li,Li Xu
In the present study, the narrow-dispersed penetrable poly(methacrylic acid- co -ethylene glycol dimethacrylate) (poly(MAA- co -EDMA)) microspheres were successfully synthesized based on the sacrificial support method. The poly(MAA- co -EDMA) microspheres mirrored the porous structure of the sacrificial support, i.e. penetrable silica, characteristic of copious mesopores and throughpores. In addition, they possessed large surface area, adjustable hydrophobicity and the cation-exchange ability. Owing to their multi functionalities, they were applied as chromatographic stationary phase to separate proteins in different separation modes, including reversed phase, hydrophobic interaction and weak cation exchange. Moreover, thanks to their throughpores, fast separation at low column backpressure could be achieved in these three modes. Both protein recovery and column stability were satisfactory. The penetrable poly(MAA- co -EDMA) microspheres were potential stationary phase matrix for fast protein separation.
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ANALYTICAL SCIENCES
·
2022
·Vol. 38
·期 1
·105-112
·
IF 1.967
Wu Xiaoxiao,Huang Jingjing,Zhang Chi,Kang Xuejun
A novel nanofiber-based solid phase extraction (NFSPE) coupled with HPLC–DAD was developed for the determination of salivary histidine, a new potential index of physiological events. The treatment of the sample was based on a coupling reaction of histidine with the diazotization products of sulfanilic acid and sodium nitrite in a slightly alkaline medium, followed by NFSPE. Nanofibers comprising polystyrene and zinc acetate were used as a novel solid-phase sorbent to extract derived histidine via the chelation of Zn 2+ with the imidazole group in the analyte. The eluted target compound was analyzed by HPLC–DAD. Good linearity was achieved with the concentrations of histidine ranging from 0.645 to 64.5 µM; the detection limit was 0.193 µM. The intra-day and inter-day coefficients of variation were less than 8.0%. The method was successfully applied to the determination of salivary histidine in the subjects exposed to a public speaking stress. Graphical abstract
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2022
·
IF 3.318
Pengqi Guo,Fanru Zhong,Yongze Zhao,Xinya Xu,Weiming Xue,Yichen Wang,Xiaoping Song,Weili Tang,Daidi Fan
In this study, a temperature-sensitive molecularly imprinted polymer was prepared by using the bifunctional monomer with the critical phase transition characteristics. Infrared spectrometry, scanning electron microscopy, and specific surface area testing were used to characterize the polymers. Then, the recognizing properties of the polymers were studied. Based on the prepared smart polymers, an SPE-HPLC analytical method for the determination of quinolizidine alkaloids in the extracts of Sophora flavescens was established and verified. Finally, the smart polymers were applied to the enrichment of quinolizidine alkaloids in plant extracts. By changing the temperature and solvents of the solid phase extraction conditions, the extraction process can increase the concentration of quinolizidine alkaloids by 4.3 to 5.2 folds. The extraction process has mild conditions and less time consumption, avoiding the use of a large number of toxic reagents, which indicate that the extraction process are more efficient and environmentally friendly.
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FOOD CHEMISTRY
·
2022
·
IF 9.231
Xiang Li,Chang-Ling Sun,Yu Xu,Shi-Hui Shan,Han Zheng,Xiao-Lu Guo,Jiang-Ning Hu
A novel method for benzo(α)pyrene (Bαp) enrichment from an oil matrix was developed by using magnetic nanoparticles (Fe 3 O 4 @dopamine/graphene oxide, Fe 3 O 4 @DA/GO) as extraction absorbents, and the chemical properties of the synthesized nanoparticles were characterized. Various parameters were investigated to optimize the extraction of Bαp from oils. Under optimal conditions (pH, 4; extraction time, 0.5 min; elution solvent, 1 mL; absorbent weight, 20 mg; elution time, 0.5 min), these nanoparticles showed excellent abilities to enrich Bαp from the saponified oil solution and were easily separated by a magnet. High-performance liquid chromatography plus fluorescence detection (HPLC-FLD) was then applied to determine the Bαp content with excellent linearity (R 2 = 0.999). The detection limit was 0.13 µg/kg, while the limit of quantification was 0.42 µg/kg. The spiked recoveries of Bαp in oils ranged from 73.5% to 121%. Compared with previous reports, the proposed method displayed many advantages, including a high efficiency of oil matrix removal, short extraction time, and convenient extraction procedure.
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MICROCHIMICA ACTA
·
2022
·Vol. 189
·期 9
·1-10
·
IF 6.408
Yang Xiao-Shuai,Zhao Jie,Wang Lu-Liang,Liu Yu-Shen,Liu Quan-Wen,Peng Xin-Yan,Wang Ping
Covalent organic framework (COF)–decorated magnetic nanoparticles (Fe 3 O 4 @DhaTab) with core–shell structure have been synthesized by one-pot method. The prepared Fe 3 O 4 @DhaTab was well characterized, and parameters of magnetic solid-phase extraction (MSPE) for parabens were also investigated in detail. Under optimized conditions, the adsorbent dosage was only 3 mg and extraction time was 10 min. The developed Fe 3 O 4 @DhaTab-based MSPE-HPLC analysis method offered good linearity (0.01–20 μg mL −1 ) with R 2 (0.999) and low limits of detection (3.3–6.5 μg L −1 ) using UV detector at 254 nm. The proposed method was applied to determine four parabens in environmental water samples with recoveries in the range 64.0–105% and relative standard deviations of 0.16–7.8%. The adsorption mechanism was explored and indicated that porous DhaTab shell provided π-π, hydrophobic, and hydrogen bonding interactions in the MSPE process. The results revealed the potential of magnetic-functionalized COFs in determination of environmental contaminants. Graphical abstract
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危险品化学品经营许可证（带存储）