JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY
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2017
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IF 3.154
Yehong Han,Chunliu Yang,Yang Zhou,Dandan Han,Hongyuan Yan
A new method involving ionic liquid–hybrid molecularly imprinted material–filter solid-phase extraction coupled to high-performance liquid chromatography (IL–HIM–FSPE–HPLC) was developed for the simultaneous isolation and determination of 6-benzyladenine (6-BA) and 4-chlorophenoxyacetic acid (4-CPA) in bean sprouts. Sample preconcentration was performed using a modified filter, with the new IL–HIM as the adsorbent, which shows double adsorption. The first adsorption involves special recognition of molecular imprinting, and the second involves ion exchange and electrostatic attraction caused by the ionic liquid. This method combines the advantages of ionic liquids, hybrid materials, and molecularly imprinted polymers and was successfully applied to determine 6-BA and 4-CPA in bean sprouts. The adsorption of 6-BA to IL–HIM is based on selective imprinted recognition, whereas the adsorption of 4-CPA is mainly dependent on ion-exchange interactions.
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TUBERCULOSIS
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2017
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IF 2.873
Shouhong Gao,Zhipeng Wang,Xinfang Xie,Chunhua You,Yang Yang,Yanhai Xi,Wansheng Chen
First-line anti-tuberculosis drugs are playing vital roles for curbing rapid spread of tuberculosis. Multidrug therapies are commonly applied in clinical to achieve better treatment outcomes. However, drug resistance and adverse reactions come along with this therapies and therapeutic drug monitoring is a feasible way to precaution them. For this reasons, a simple and sensitive method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) and single protein precipitation was developed and validated for simultaneously quantifying of pyrazinamide, isoniazid, ethambutol , streptomycin and rifampicin in human plasma. Optimized chromatographic separation was achieved on a ZORBAX SB-C 18 column with heptafluorobutyric acid, an ion-pair reagent, in the mobile phase at a flow rate of 0.3 mL/min. The mass detection was achieved using electrospray ionization in the positive ion mode with a multiple reaction monitoring mode. The lower limit of quantification (LLOQ) and dynamic range of pyrazinamide, isoniazid, ethambutol, streptomycin and rifampicin were 200–4000 ng/mL, 80–2000 ng/mL, 0.2–1000 ng/mL, 2000–200000 ng/mL and 200–4000 ng/mL, respectively. The Inter-day and intra-day accuracy and precision were within ±15.0% and less than 15%. The method had been successfully applied to simultaneous determination of four first-line Anti-tuberculosis drugs in plasma from tuberculosis patients.
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CARBOHYDRATE RESEARCH
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2015
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IF 1.929
Zhangrun Han,Yangyang Zeng,Hong Lu,Lijuan Zhang
Chitin is one of the most abundant polysaccharides on earth. It consists of repeating β-1,4 linked N-acetylated glucosamine (A) units. Chitosan is an N-deacetylated product of chitin. Chitosan and its derivatives have broad medical applications as drugs, nutraceuticals , or drug delivery agents. However, a reliable analytical method for quality control of medically used chitosans is still lacking. In current study, nitrous acid was used to cleave all glucosamine residues in chitosan into 2,5-anhydromannose (M) or M at the reducing end of di-, tri-, and oligosaccharides . PMP , i.e. 1-phenyl-3-methyl-5-pyrazolone, was used to label all the Ms. Online UV detection allowed quantification of all M-containing UV peaks whereas online MS analysis directly identified 11 different kinds of mono-, di-, tri-, and oligosaccharides that correlated each oligosaccharide with specific UV peak after HPLC separation. The DA (degree of acetylation) for chitosans was calculated based on the A/(A+M) value derived from the UV data. This newly developed method had several advantages for quality control of chitosan: 1. the experimental procedures were extensively optimized; 2. the reliability of the method was confirmed by online LC-MS analysis; 3. the DA value was obtainable based on the UV data after HPLC analysis, which was comparableto that of 1 H NMR and conductometric titration analyses; 4. finally and most importantly, this method could be used to obtain the DA as well as chemical acetylation/deacetylation mechanisms for chitosan by any laboratory equipped with a HPLC and an online UV detector.
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INTERNATIONAL JOURNAL OF MOLECULAR SCIENCES
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2013
·Vol. 14
·期 11
·21202-21214
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IF 2.464
Shengsheng Zhu,Xiang Meng,Xin Su,Yongwei Luo,Zuyue Sun
An isocratic, sensitive and stability-indicating high performance liquid chromatographic (HPLC) method for separation and determination of the related substances of micafungin sodium was developed. The chromatographic separation was achieved on Agilent Zorbax SB-C18 column (250 × 4.6 mm, 5 μm). Forced degradation study confirmed that the newly developed method was specific and selective to the degradation products. The performance of the method was validated according to the present ICH guidelines for specificity, linearity, accuracy, precision and robustness. Regression analysis showed correlation coefficient value greater than 0.999 for micafungin sodium and its six impurities. Limit of detection of impurities was in the range of 0.006%–0.013% indicating the high sensitivity of the newly developed method. Accuracy of the method was established based on the recovery obtained between 98.2% and 102.0% for all impurities. RSD obtained for the repeatability and intermediate precision experiments, was less than 1.0%. The method was successfully applied to quantify related substances of micafungin sodium in bulk drugs.Keywords:micafungin sodium;related substances;stability-indicating;forced degradation;validation
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RSC Advances
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2016
·Vol. 6
·期 111
·109730-109741
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IF 3.289
Yi Tao,Dandan Su,Yingshan Du,Weidong Li,Baochang Cai,Liuqing Di,Liyun Shi,Lihong Hu
Tyrosinase is the rate-limiting enzyme for controlling the production of melanin. A very precise, sensitive and convenient solid-phase extraction based approach was developed for extract and analysis of tyrosinase binders from San-Bai decoction. Tyrosinase binders were captured by using tyrosinase conjugated magnetic beads. The retained tyrosinase binders were dissociated and analyzed by high performance liquid chromatography and quadrupole-time-of-flight mass spectrometry. The powder X-ray diffraction (XRD), transmission electron microscopy (TEM), vibration sample magnetometer (VSM) and Fourier transform infrared (FT-IR) spectroscopy techniques were used for the characterization of tyrosinase conjugated magnetic beads. A variety of experimental conditions such as incubation temperature, buffer pH and ion strength, which may affect extraction yield, were optimized through Box–Behnken statistical design and response surface methodology by using paeoniflorin as a model compound. The optimal incubation conditions were as follows: wash times: 4, wash solvent: 10% acetonitrile–water, incubation time: 30 min, temperature: 34.84 °C, ion strength: 193.67 mM, pH: 6.98. The established approach was successfully applied for the extraction of tyrosinase binders from San-Bai decoction. The tyrosinase inhibitory assay was employed for validation of the activities of these identified binders. Fifteen tyrosinase inhibitors were identified, and nine of which, including benzoylpaeoniflorin, benzoyloxypaeoniflorin, galloylpaeoniflorin, paeonolide, oxypaeoniflora, albiflorin, ononin, mudanpioside C and apiopaeonoside, were reported for the first time.
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FOOD CHEMISTRY
·
2024
·
IF 8.5
Xiaojiao Zheng,Xingle Guo,Yawen Zhang,Jiajun Han,Xu Jing,Junxue Wu
A novel, environmentally friendly, and efficient method for determining triazine herbicides in water, tea, and juice was developed by combining magnetic dispersive micro-solid phase extraction (MD-μSPE) with magnetic dispersive liquid-liquid microextraction (MDLLME), followed by high-performance liquid chromatography (HPLC). The pretreatment process, utilized magnetic biochar (MBC) and magnetic deep eutectic solvent (MDES) as the adsorbent and extractant, respectively. Fe(NO 3 ) 3 was loaded onto waste mushroom sticks to prepare MBC via impregnation-pyrolysis, while tri- n -butylphosphine oxide, nonanoic acid, and FeCl 3 were combined through hydrogen bonds to form MDES. This approach significantly reduced environmental impact using waste materials and shortened separation times. The method demonstrated excellent linearity (1–100 μg L −1 ), low detection limits (0.3 μg L −1 ), and good precision (RSDs <6.5 %). Recoveries in water, tea, and juice ranged from 80.1 % to 90.6 %. This combined MD-μSPE-MDLLME approach offers a greener and more efficient extraction process for separating and concentrating pesticides from complex food samples.
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Phytochemistry Letters
·
2024
·
IF 1.3
Yu-Fei Hou,Lu Bai,Shao-Jing Liu,Sen Guo,Ya-Long Wang,Chi-Tang Ho,Nai-Sheng Bai
A. arguta leaves, as an important by-product during the ripening of A. arguta fruits, are usually discarded. It contains numerous flavonoid components. In the present research, a simple and reproducible HPLC-DAD method was established and verified for simultaneous identification and quantification analysis of 25 flavonoid components in A. arguta leaves. The findings indicated that the highest concentration of flavonoid compounds in A. arguta leaves was quercetin ( 2 ), with a content of 8.97 ± 0.09 mg/g. The content of flavonoids in samples from different cultivation bases was different, indicating that the varied flavonoid contents are possibly determined by geographical variance. This method can be used for the quality control of Actinidia arguta . The 25 flavonoids showed good α-glucosidase inhibitory activity with IC 50 values ranging from 0.35 to 4.15 mM, and the activity difference varied with the different structures. 2"- O -galloylhyperin ( 18 ) showed the best antihyperglycemic action (IC 50 = 0.35 ± 0.01 mM), followed by quercetin ( 2 , IC 50 = 0.38 ± 0.01 mM), quercetin 4′- O -galactoside ( 19 , IC 50 = 0.41 ± 0.01 mM), kaempferol ( 3 , IC 50 = 0.42 ± 0.01 mM), and kaempferol-3-rutinoside ( 6 , IC 50 = 0.53 ± 0.01 mM). Molecular docking analysis demonstrated that the interaction modes of these five stronger inhibitors with α-glucosidase were mainly hydrogen bonding and hydrophobic interaction. The results showed that compounds with different structural skeletons interacted with different amino acid residues and exerted different degrees of α-glucosidase inhibition. Therefore, A. arguta leaves and their flavonoids may be beneficial against diabetes, and higher levels of flavonoids are considered to have greater potential for medicinal use.
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FOOD CHEMISTRY
·
2024
·
IF 8.5
Ruidong Zhou,Cong Kong,Yupeng Wen,Guangxin Yang,Wendi Huo,Chaoying Zhang,Huiwu Sun,Huan Liu,Dongmei Huang,Jincheng Li
A 15-channel pressure filtration purification method was presented for high throughput sample preparation of aquatic products. A cost-effective device was constructed and melamine sponge was selected as the cleanup sorbent. Upon interfacing with HPLC-MS/MS, the analytical procedure demonstrated its suitability for quantifying 160 pesticides and veterinary drug residues in aquatic products such as fish, shrimp, and crab. The method achieved sample recoveries ranging from 61.3 to 124.9 %. The detection limits were established between 0.5 and 1.0 μg/kg, while the quantitation limits were confirmed to be within the range of 1.0–2.0 μg/kg. The method was applied to quantify the pesticide and veterinary drug residues in mostly consumed aquatic products from five coastal provinces in China. The results showed significant differences between different aquatic products in the concentrations of pesticide and veterinary drug residues, implying the necessity of supervision for the accurate determination of pesticides and veterinary drugs.
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PHYTOCHEMICAL ANALYSIS
·
2024
·
IF 3
Yangfei Wei,Tao Chen,Hai Song,Shuo Wang,Cheng Shen,Xiaojun Wang,Yulin Li,Junke Wang
Introduction Screening of novel pancreatic lipase inhibitors from complex natural products is a meaningful task. Objectives Through accurately screening and separating pancreatic lipase inhibitors from Clematis tangutica ( C. tangutica ), to discover new leading compounds for slimming and accelerate the development and utilization of Tibetan medicine resources. Methods An integrated strategy that combines affinity ultrafiltration and high-performance liquid chromatography-quadrupole time-of-flight mass spectrometry (AU-HPLC-QTOFMS), targeted separation, in vitro validation, and molecular docking was developed to screen pancreatic lipase inhibitors from C. tangutica . The AU-HPLC-QTOFMS technique was performed to fish for the potential active substances. Macroporous resin, preparative liquid chromatography, and high-speed countercurrent chromatography were implemented for the accurate and targeted separation of active compounds. The inhibitory activities of target compounds to pancreatic lipase were detected by the inhibition experiments in vitro. The binding affinities and binding sites were analyzed using molecular docking. Results A total of eleven kinds of pancreatic lipase inhibitory substances were screened from C. tangutica . Seven triterpenoid saponins were screened for the first time as lipase inhibitors and successfully prepared with purities higher than 97%. Tanguticoside B, clematangoticoside J, hederoside H 1 , and rutin showed stronger inhibitory effects with IC 50 values of 1.539 ± 0.048, 1.661 ± 0.092, 1.793 ± 0.069, and 1.792 ± 0.094 mmol/l. Moreover, they have the lowest ΔG values of −10.84, −9.97, −10.87, and −9.39 kcal/mol to pancreatic lipase. Conclusion The integrated strategy using AU-HPLC-QTOFMS, targeted separation, in vitro validation, and molecular docking was feasible for rapidly screening and directionally isolating pancreatic lipase inhibitors from C. tangutica .
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JOURNAL OF CHROMATOGRAPHY A
·
2025
·
IF 4
Qianyu Wu,Yu Zhang,Ce Sun,Jun Dang
In this study, we developed an online HPLC-lipoprotein lipase system capable of directly recognizing chromatographic peaks corresponding to lipoprotein lipase affinity agents from Nitraria tangutorum . Notably, using the HPLC-lipoprotein lipase system, six lipoprotein lipase affinity agents were successfully recognized and isolated with purities > 95 %, including one phenylpropanoid, one apigenin, and four quercetin derivatives. In vitro enzymatic assays and molecular docking studies demonstrated that these glycosylated compounds bind effectively to the active site of lipoprotein lipase, with binding energies ranging from -7.2 to -8.8 kcal/mol. The compounds also showed notable affinity, with median inhibitory concentration values between 56.2 μM and 202.3 μM and half-maximal effective concentration values ranging from 106.8 μM to 311.0 μM. These results suggest that quercetin glycosides in Nitraria tangutorum contribute significantly to the regulation of lipoprotein lipase activity. Importantly, the established online HPLC-lipoprotein lipase recognition system demonstrated broad application prospects, particularly by providing a rapid and high-precision method for discovering lipoprotein lipase affinity agents in chemically complex natural products.
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MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Dan Li,Zhiqin Huang,Jing Lin,Laisheng Li
a new bis (5-chloro-2,4-dimethoxyphenylureido)-β-cyclodextrin stationary phase (MOCDP) was prepared via the reaction of mono -6-ethylenediamino-β-cyclodextrin with reactive isocyanate, and immoblization proccess. After characterization, MOCDP was used to resolve triazole pesticides, and we found that it had strong separation abilities for various triazoles ( R s = 1.42 ∼ 2.72). Especially, it could completely separate triazoles with two chiral centers into four enantiomers for the first time. Through optimizing the gradient elution program with ACN/MeOH/H 2 O, total ten triazole enantiomers ( R s = 1.75 ∼ 3.84) were simultaneously separated, including two hexaconazole, four triadimenol, and four metconazole enantiomers. Based on MOCDP column, a new HPLC method for the simultaneous quantification of the above ten residual triazole pesticide enantiomers in five fruits and vegetables (tomatoes, cucumbers, green peppers, apples, and bananas) was established with internal standard method and PDA detector at 220 nm. The elution order was triadimenol A (SR-,RS-) > triadimenol B (RR-,SS-) > hexaconazole (R-,S-) > metconazole A (RS-,SR-) > metconazole B (RR-,SS-). The good linear relationship ( R 2 = 0.9959 ∼ 0.9993) was observed in the range of 0.5 ∼ 50 mg/L (triadimenol B and metconazole B enantiomers) and 1.0 ∼ 100 mg/L (other enantiomers). The average recoveries of enantiomers were 82.58 %∼104.21 % ( n = 15) with the RSDs of 1.55 %∼3.97 % ( n = 5, intra -day) and 1.98 %∼4.42 % ( n = 15, inter -day). The limits of detection and quantification were 0.03 ∼ 0.05 mg/kg and 0.10 ∼ 0.15 mg/kg, respectively. The chiral separation mechanism was also discussed through molecular simulation, revealing that the driving forces should be hydrogen bond, π-π stacking and inclusion complex derived from bisphenylureido groups and CD moiety in the chiral separations. This internal standard method had characterization of simple pretreatment, accurate quantification, and low cost.
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ACS Food Science & Technology
·
2025
·
IF 2.8
Yan Cui,Lin Zhu,Haitao Shang,Xiaoting Xuan,Xudong Lin,Shanqiao Chen
This research characterized the nonvolatile and volatile flavor compounds of five representative honey peach cultivars (Chiyue, Hujingmilu, Baili, Liangfang, and Yulu) from Fenghua City using HPLC and GC-IMS, coupled with multivariate analysis. Total soluble solids (TSS), titratable acid (TA), TSS/TA ratio, pH, and total phenolic content varied significantly among cultivars. Liangfang had the highest sugar levels, contributing to its elevated sweetness. A total of 33 volatiles were identified, with ethyl acetate, hex-2-enal, and hexanal dominating. The cultivars were grouped into three clusters based on their volatile profiles. Thirteen key aroma compounds (relative odor activity value >1) were identified. Chiyue and Hujingmilu had high levels of limonene and isobutyl acetate, while Baili exhibited green notes from hex-2-enal and 2-methylbutanal. Yulu showed the highest levels of (E)-2-hexenyl acetate, ethyl hexanoate, ethyl 2-methylbutyrate, hexanal, and linalool with fruity, green, and floral aromas. This research provides insights for peach flavor analysis and breeding.
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危险品化学品经营许可证（带存储）