TALANTA
·
2016
·
IF 4.035
Xixi Wang,Xueying Li,Xiaoya Jiang,Peipei Dong,Haiyan Liu,Ligai Bai,Hongyuan Yan
A high performance liquid chromatography (HPLC) monolithic column was prepared by redox polymerization of styrene , dipentaerythritol hexaacrylate (DPHA) and ethylene glycol dimethacrylate (EDMA) in a porogen system of n-propanol/PEG400. The monolith was characterized by scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and the results indicated that the monolith had a stable and homogeneous structure. The porosity of the monolithic column was 75.86% and average pore diameter was 2.1 µm. Several alkylbenzenes and anilines were used to evaluate the column performance in terms of hydrophobicity . Then the column was applied to separate small molecules including phytosterol and BSA tryptic digest. Finally, five standard proteins, egg white and plasma were separated respectively and high separation capacity of protein was obtained.
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JOURNAL OF CHROMATOGRAPHY A
·
2016
·
IF 3.926
Xiao-Fei Gu,Yue Zhao,Kan Li,Meng-Xiang Su,Fang Yan,Bo Li,Ying-Xiang Du,Bin Di
Structure elucidation of volatile aromatic isomers at trace level has long been considered as an elusive task, due to their structural similarities and similar polarities, even with the aid of many spectroscopic techniques such as mass spectrometry and nuclear magnetic resonance (NMR) spectroscopy. Single-crystal X-ray diffraction (SCD) is recognized as one of the most powerful structural elucidation techniques. The recently developed crystalline sponge method overcomes the intrinsic limitation of SCD that the target molecules must be single crystals, being able to analyze non-crystalline and trace-amount compounds without any special treatment. In order to investigate whether the crystalline sponge method could be used for the structure elucidation of closely related isomers or other volatile and even oily compounds in complex mixtures at trace level, we combined HPLC separation with the crystalline sponge method for X-ray crystallographic analysis. In this paper, two pairs of volatile aromatic isomers including cis / trans isomers of asarone and positional isomers of carvacrol and thymol, as well as the main volatile component in essential oil extracted from Acorus Tatarinowii , were first isolated by HPLC and encapsulated into the crystalline sponge then elucidated by X-ray crystallographic analysis. Direct observation of these volatile compounds by X-ray crystallography was achieved using only microgram quantities without crystallization or derivatization. Unambiguous identification of these compounds was realized without reference standards. This strategy offers a promising platform capable of providing high-confidence detailed structural information of closely related isomers as well as other volatile and even oily compounds in complex mixtures in microgram quantities.
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ANALYTICAL LETTERS
·
2025
·
IF 1.8
Wanying Zhao,Yanqin Chen,Jun Tan,Yanru Bai,Fudong Ma
A method utilizing high-performance liquid chromatography with evaporative light scattering detection (HPLC-ELSD) has been developed and validated for the simultaneous determination of raffinose, glucose, sucrose, and stachyose in waste liquid from cottonseed processing and in byproducts including cottonseed meal. The separation was performed using a carbohydrate ES column (250 × 4.6 mm, 5 μm) and isocratic elution with acetonitrile and water (70:30, v/v). The temperature of the column oven was maintained at 35 °C. The drift tube temperature for evaporative light scattering detection (ELSD) was operated 40 °C, while the nitrogen flow was set to 1.5 L·min−1. The saccharides were separated by HPLC-ELSD within 20 min. The coefficients of determination (R2 = 0.9986–0.9999) indicate that there was a linear relationship between saccharides and the response. The limits of detection were 0.004–0.023 mg·mL−1 and the quantification range was from 0.013 to 0.080 mg·mL−1. The intraday and interday precision were from 0.05 to 0.55% and 0.20 to 0.58%, respectively. The recovery was from 102.75 ± 2.03% to 106.76 ± 2.09% and the relative standard deviations were 1.87 to 1.98%. The method exhibited good stability in determining four saccharides in cottonseed processing waste liquid and the resultant byproduct cottonseed meal. This method exhibits high separation efficiency and sensitivity, excellent precision, and simplicity, which allows determination of the high value-added product, raffinose, in cottonseed processing waste liquid and meal.
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LWT-FOOD SCIENCE AND TECHNOLOGY
·
2024
·
IF 6
Dan Wei,Qiao Deng,Jianliang Li,Jingjing Xu,Ming Guo,Huizhen Wu,Ju Zhang,Jianchang Jin,Xu Wang
Mycotoxins co-contamination in soybean poses great risks to human health, however, due to their diverse structures, it is difficult to simultaneously extract and detect these multi-mycotoxins. By incorporating modification of hydrophilic carboxyl groups with the hydrophobic properties of covalent organic frameworks, a stable cubic carboxyl-functionalized magnetic amide-linked covalent organic framework were fabricated, characterized and utilized as adsorbents for magnetic solid phase extraction (MSPE) of eleven frequently detected mycotoxins from soybeans followed by HPLC-MS/MS analysis. The key MSPE parameters were screened using the Plackett-Burman design and optimized with the Box-Behnken design for response surface methodologies. Under the optimal experimental conditions, the linear range was 0.2–50 μg/kg, the limits of detection were 0.1–1.4 μg/kg. The established method was applied for the soybean analysis with satisfactory recoveries (70.8–108.3%) and precision (intra- and inter-relative standard deviations of 2.1–9.2% and 1.6–11.1%, respectively). With proper modification, this method may have great application potential for simultaneously analyzing and monitoring the multi-mycotoxin contamination in foods to ensure consumer safety and public health.
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TALANTA
·
2024
·
IF 5.6
Shurong Chen,Min Zhu,Ying Wang,Jinru Ding,Mingji Tan,Jindou Zhao,Jiahan Xie,Zhibing Wang
A novel temperature-responsive supramolecular solvent was prepared with cetyltributylphosphonium tetrafluoroborate and sodium citrate. It served as the extraction solvent of dispersive liquid-liquid microextraction for the extraction and enrichment of pyrethroids in tobacco samples. In this study, the preparation of the temperature-responsive supramolecular solvent and the extraction of the target analytes were integrated into one step, which simplified the experimental process. Due to the low melting point of the prepared supramolecular solvent, the traditional liquid-liquid separation can be converted to solid-liquid separation at low temperatures. This conversion facilitates precise collection of the supramolecular solvent and reduces the loss of target analytes. The composition, structure, physicochemical properties, and micromorphology of the supramolecular solvent were characterized. The formation and extraction mechanism of supramolecular solvent were explored, and the extraction conditions were optimized. The results indicated that good linearity of target analytes ( R 2 > 0.9998) was obtained within the linear range. The limits of detection and quantification for the five pyrethroids were in the range of 0.25–0.50 μg L −1 and 0.85–1.65 μg L −1 , respectively. The present method can be used for the analysis of pyrethroid pesticide residues in tobacco samples.
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JOURNAL OF SEPARATION SCIENCE
·
2017
·Vol. 40
·期 20
·4032-4040
·
IF 2.557
Qingxiang Zhou,Yongyong Yuan,Yalin Wu,Yongli Liu
A novel magnetic core–shell material polyaniline@SiO 2 @Fe (PANI@SiO 2 @Fe) has been successfully synthesized and investigated as an effective adsorbent for the magnetic solid-phase extraction of typical endocrine disrupting compounds such as bisphenol A, tetrabromobisphenol A, and 4-nonylphenol from water samples. The morphology of the as-prepared PANI@SiO 2 @Fe was characterized by transmission electron microscopy and X-ray diffraction. The main parameters that influenced the enrichment performance such as the kind of eluent, amount of adsorbent, volume of eluent, adsorption time, elution time, ionic strength, pH, concentration of humic acid, and sample volume were investigated. Under the optimal conditions, a good linear relationship was found in the range of 0.05–100 μg/L for bisphenol A, 0.05–300 μg/L for tetrabromobisphenol A, and 0.05–250 μg/L for 4-nonylphenol, respectively. The correlation coefficients are all above 0.995. The limits of detection were in the range of 0.009–0.04 μg/L, and precisions were under 3.73% ( n = 6). The real water analysis indicated that the spiked recoveries were in the range of 92.9–98.9% ( n = 3). All these results indicated that the developed method was an efficient tool for the analysis of bisphenol A, tetrabromobisphenol A, and 4-nonylphenol.
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Analytical Methods
·
2018
·Vol. 10
·期 11
·1325-1330
·
IF 2.073
Yong Zhang,Zhizhong Zou,Guixing Chou
To quickly determine the amounts of kirenol, darutoside and darutigenol in Herba Siegesbeckiae using HPLC, the efficiency of sample cleanup with different solid phase extraction methods was systematically investigated. The results showed that a polymer based strong anion exchange (P-SAX, 200 mg/6 mL) sorbent could separate and enrich diterpenoids providing rapid determination without impurity interference. In this paper a new HPLC-UV method using a core–shell column (Boltimate C18 3.0 × 100 mm, 2.7 μm) for the quantitative determination of three diterpenoids was developed. Under optimum experimental conditions, P-SAX pretreatment with a core–shell analytical column exhibited satisfactory results in the determination of diterpenoids in Herba Siegesbeckiae with recovery rates of 95–102%, relative standard deviations below 1.1%, a limit of quantitation as low as 0.1 6 μg mL−1, and a short analytical runtime of 8 min. Finally, the proposed method was successfully applied in the profiling of diterpenoids in Herba Siegesbeckiae from different regions.
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JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2024
·
IF 1.5
Zhang Chenxia,Wu Zeyi,Qiu Meiyan,Li Yanhua,Wang Zhongqing,Fan Xiaomei,Cai Shaoyu,Rao Wanbing
The difficulty on determination of high boiling point solvents, always exist due to their low vapor pressure in headspace (HS) vial. What’s worse, the commonly used GC diluents, such as N, N-dimethylacetamide, 1,3-dimethyl-2-imidazolidinone, dimethyl sulfoxide, N, N-dimethylformamide and N-methylpyrrolidone are often remained in HS instrument after frequent injection into HS, thus would result in terrible positive interference problem. In this work, a fast and sensitive HPLC method in combination with a sample precipitation method, was proposed for the determination of above five high boiling point solvents in drug substances within 14.5 min. The final method was validated with regard to limit of detection and limit of quantitation, precision, linearity and accuracy in accordance with ICH Q2 (R1). Finally, the proposed strategy was successfully applied for the analysis of high boiling point solvents used in three active pharmaceutical ingredients. The established generic strategy would provide another choice for the determination of high boiling point solvents in pharmaceuticals.
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2024
·
IF 4
Xu Ling,Yifan Hu,Yiming Hu,Jingwen Meng
Research about mulberry leaf with different producing area and harvest period will promote its quality control method and utilization in terms of active ingredient extraction and health products research. This study focused on the establishment of fingerprint of mulberry leaves from different harvest periods and different origins, the determination of chlorogenic acid , rutin as well as astragalin with ultrasound assisted liquid extraction. The extraction rate was optimized using response surface method . The optimized conditions were as follows: methanol for extraction, ultrasonic power of 240 W, extraction time of 77 min, methanol concentration of 59 % (v/v) and solid-to-liquid ratio of 1:48 (g/mL). Three ingredients in mulberry leaves were successfully extracted, and the HPLC fingerprint of mulberry leaves was established with 23 common peaks. Good similarity higher than 85.7 % was obtained among the 14 batch of samples from different harvest periods and different origins. The optimized extraction process was stable, reliable and suitable for extracting chlorogenic acid and two flavonoids from mulberry leaf. The established fingerprint exhibited good stability and repeatability, and provided comprehensive chromatographic peaks information. This method can be relied upon for the identification and comprehensive quality control of mulberry leaf.
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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES
·
2024
·
IF 1
Xiang-Jun Tu,Guang-Wen Fan,Xiang Ji,Ze-Xu Pan,Han Meng,Yu-Li Sang,Yan-Jun Hao,Nan Liu
Ganmaoling Granule (GMLG) is one of the most effective Chinese Patent Medicines (CPMs) which is applied to relieve the uncomfortable symptoms caused by the common cold. In this study, high-performance liquid chromatography (HPLC) combined with chemometric analyses and multi-component content determination were performed to preliminary investigate the effect of ozone sterilization technology on the quality of GMLG. The methodology validation and similarity analysis results showed that the analytical method was capable of complying with the demand of HPLC fingerprints, and 80 batches of GMLGs before and after ozone sterilization in four process stages had a high degree of similarity based on the values of similarity analysis (SA) was greater than 0.98. The results of hierarchical cluster analysis (HCA) and principal component analysis (PCA) showed that the GMLGs before and after ozone sterilization were divided into two categories, and the same batch of GMLGs was clustered into the same group. Meanwhile, the contents of linarin, caffeine, chlorpheniramine maleate and acetaminophen between 24 batches of GMLGs before and after ozone sterilization had no statistically significant differences (P > 0.05), which met the requirements of “Drug Standard of the People’s Republic of China”. In conclusion, the ozone sterilization technology had no obvious influence on the quality of GMLGs in four process stages, which provided a reference for the quality control of GMLG and other Chinese-western medicine compound preparations.
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TALANTA
·
2024
·
IF 5.6
Zi-Yu Li,Jia-Hui Zhu,Jie Zhao,Xiao-Shuai Yang,Yu-Shen Liu,Ting Cheng,Yan-Xin Chen,Shu-Yang Sun,Lu-Liang Wang
Magnetic solid-phase extraction (MSPE) technology for tetracycline (TCC) was developed by employing the novel and pre-designed Fe 3 O 4 –COOH@hydrogen-bonded organic frameworks (HOFs) adsorbents in complex food samples. The HOF shell was grown onto the Fe 3 O 4 –COOH core by in-situ self-assembled method. The excellent MSPE performances with less solvent, less adsorbent and time consumption were derived from the hydrogen bonding, π-π and hydrophobic interactions between HOF shell and TCC. Combined with HPLC analysis, Fe 3 O 4 @ HOFs adsorbent reduced matrix effects and the established MSPE-HPLC method for TCC gave the linearity of 0.001–6 μg mL −1 with the limit of detection 0.0003 μg mL −1 . The recoveries in pure milk, canned yellow peach and carrot were 82.4–103.7 %. The method provided a simple, efficient and dependable alternative to monitor trace TCC antibiotics in food or environmental samples.
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MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Jianjin Guo,Chi-Tang Ho,Naisheng Bai
This comprehensive study utilized response surface methodology (RSM) to optimize extraction conditions for total flavonoids and phenols from F. mandshurica . Optimal conditions for flavonoids were 75 % ethanol, 63 °C, and 84 min, yielding 14.98 ± 0.13 mg/g. For phenols, it was 70 % ethanol, 66 °C, and 87 min, resulting in 26.04 ± 0.22 mg/g. UPLC-Q-TOF-MS/MS identified 68 constituents in F. mandshurica , categorized into groups. HPLC-DAD established a method for quantitative analysis of 12 target compounds. Geographical distribution analysis highlighted the northeast region as the main production area. Fingerprinting of 30 samples and multivariate analysis identified five active compounds. Hierarchical cluster analysis (HCA) showed differences in active compounds based on origin. In vitro antidiabetic evaluation demonstrated α-glucosidase inhibitory effects. Molecular docking studies were conducted between 12 active compounds and the antidiabetic-related protein 8A27. Esculetin had the highest binding affinity. The study examined extraction methods, analyzed samples, and explored antidiabetic effects, providing data support and insights for F. mandshurica as a natural industrial product and for extracts and active compounds as antidiabetic sources.
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