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FOOD CHEMISTRY · 2021 · IF 7.514

Collaborative compounding of metal–organic frameworks for dispersive solid-phase extraction HPLC–MS/MS determination of tetracyclines in honey

Yue-Hong Pang,Zhi-Yang Lv,Ji-Cheng Sun,Cheng Yang,Xiao-Fang Shen

Metal-organic frameworks (MOFs), a sort of dispersive solid-phase extraction (d-SPE) material, has shown considerable prospects in the pretreatment of food, biological and other complex samples. Herein, we developed a method for compounding MOFs for d-SPE and trace determination of tetracyclines (TCs) in honey. When the compounding ratio of MIL-101 (Cr), MIL-100 (Fe) and MIL-53 (Al) was 7:1:2, adsorption–extraction was effective. Followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS), the limits of detection were 0.073–0.435 ng/g and the limits of quantitation ranged from 0.239 to 1.449 ng/g for oxytetracycline, tetracycline, chlortetracycline and doxycycline. The method was applied to four kinds of honey samples with recoveries from 88.1% to 126.2%. The compounding of MOFs provides a strategy for purification and multi-target extraction from complex food matrices by d-SPE.

研究领域: 分析化学 · 食品安全
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JOURNAL OF FOOD COMPOSITION AND ANALYSIS · 2022 · IF 4.52

Simultaneously quantification of organic acids metabolites by HPLC mass spectrometry to reveal the postharvest quality change in cherry tomato

Meng Dong,Ran Xin,Zhi-Yuan Li,Yu-Lian Li,Xu-Hui Huang,Xiu-Ping Dong,Bei-Wei Zhu,Lei Qin

The organic acids in fruits have critical impacts on palatability and flavor . In this paper, we established a method to quantify 21 essential organic acids in animal and plant matrices using HPLC mass spectrometry with high sensitivity and broad applicability. The organic acids in 12 animal and plant matrices were quantified. Additionally, the profile and concentration of organic acids could achieve the classification of samples. The fruit quality traits and important organic acids content during the storage of cherry tomatoes were monitored via our method. Nine organic acids changed significantly in 16 days of storage, especially citric acid , as the most predominant organic acid, decreased from 4260 to 2290 μg/g, leading to a decline in sourness of 46.2 %. In contrast, after 16 days of storage, galacturonic, gluconic, malonic and quinic acids increased by 155 %, 88 %, 162 %, and 112 %, respectively, which had a potential effect on softening and deteriorating of cherry tomatoes.

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Food Chemistry-X · 2023 · IF 6.1

Aqueous two-phase systems coupled with chemometrics-enhanced HPLC-DAD for simultaneous extraction and determination of flavonoids in honey

Xiao-Hua Zhang,Xiang-Dong Qing,Jing-Jing Zheng,Yan Yu,Jiaojiao Huang,Chao Kang,Zhi Liu

In this study, an accurate, rapid, green, and environment friendly method for the extraction and quantitative analysis of flavonoids in honey was established by using the aqueous two-phase extraction combined with the chemometrics-assisted HPLC-DAD. The first purpose of this study was to extract seven flavonoids in five different types of honey using alcohol/salt aqueous two-phase system (ATPS). The system with 2.82 mL sodium citrate (30%), 1.58 mL water, and 3.10 mL isopropanol, showed the highest flavonoids extraction yields in the top phase (87.66–101.50%). Additionally, the three-way array of honey samples based on HPLC-DAD was decomposed mathematically by the alternating trilinear decomposition (ATLD) algorithm to obtain reasonable chromatograms, spectra, and concentration profiles for each analyte. Compared with the traditional solid-phase extraction method, the ATPS-ATLD-based method showed satisfactory spiked recoveries, lower limit of detection, and higher sensitivity, further verifying its accuracy and stability.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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Analytical Methods · 2022 ·Vol. 14 ·期 25 ·2522-2530 · IF 3.532

A novel magnetic metal–organic framework absorbent for rapid detection of aflatoxins B1B2G1G2 in rice by HPLC-MS/MS

Ling-Juan Wang,Zhi-Wei Chen,Teng-Zhou Ma,Jiang Qing,Fang Liu,Zhou Xu,Ye Jiao,Shi-Hua Luo,Yun-Hui Cheng,Li Ding

In this study, a core–shell-structured magnetic metal–organic framework (MMOF) composite material (Fe3O4@UiO-66-NH2) was synthesized by the solvothermal method. It was employed as a new absorbent in combination with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for the simultaneous detection of four aflatoxins (AFs) in rice. This method could shorten the pre-processing time by exploiting the advantageous characteristics of magnetic cores. The impurity was removed quickly. The effects of extraction solution, extraction time, adsorbent types, and amount of adsorbent on the extraction rate of target compounds were optimized. Under optimized conditions, AFs were validated and showed a good linear relationship within the 0.375–20 μg kg−1 concentration range (r2 > 0.9992). The limit of detection (LOD) was 0.0188–0.1250 μg kg−1 and the limit of quantification (LOQ) was 0.0375–0.3750 μg kg−1. At three spiking levels (0.375, 2, and 10 μg kg−1), the average recovery values for the four AFs ranged from 85.1% to 111.0%. The relative standard deviation ranged from 3.4% to 7.7%. The new method proved to be simple, fast, efficient, and suitable for the determination of AFs in rice samples.

CAS / MDL: 10025-77-1
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Pharmaceuticals · 2021 ·Vol. 14 ·期 11 ·1194 · IF 5.863

Simultaneous Quantification of Propylthiouracil and Its N-β-d Glucuronide by HPLC-MS/MS: Application to a Metabolic Study

Min Li,Qingfeng He,Li Yao,Xiaofeng Wang,Zhijia Tang,Xiao Zhu,Hai-Shu Lin,Xiaoqiang Xiang

Propylthiouracil (PTU) is commonly prescribed for the management of hyperthyroidism and thyrotoxicosis. Although the exact mechanism of action is not fully understood, PTU is associated with hepatoxicity in pediatric population. Glucuronidation mediated by uridine 5′-diphospho-glucuronosyltransferases (UGTs), which possess age-dependent expression, has been proposed as an important metabolic pathway of PTU. To further examine the metabolism of PTU, a reliable HPLC-MS/MS method for the simultaneous quantification of PTU and its N-β-D glucuronide (PTU-GLU) was developed and validated. The chromatographic separation was achieved on a ZORBAX Extend-C18 column (2.1 × 50 mm, 1.8 μm) through gradient delivery of a mixture of formic acid, methanol and acetonitrile. The electrospray ionization (ESI) was operated in its negative ion mode while PTU and PTU-GLU were detected by multiple reaction monitoring (MRM). This analytical method displayed excellent linearity, sensitivity, accuracy, precision, recovery and stability while its matrix effect and carry-over were insignificant. Subsequently, the in vitro metabolism of PTU was assessed and UGT1A9 was identified as an important UGT isoform responsible for the glucuronidation of PTU. The information obtained from this study will facilitate future mechanistic investigation on the hepatoxicity of PTU and may optimize its clinical application.Keywords:propylthiouracil;propylthiouracil glucuronide;in vitro;human liver microsomes;UGT1A9;HPLC-MS/MS

CAS / MDL: 51-52-5
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2021 ·Vol. 10 ·期 11 ·2814 · IF 4.35

Simultaneous Determination of Purines and Uric Acid in Chinese Chicken Broth Using TFA/FA Hydrolysis Coupled with HPLC-VWD

Manli Wu,Wangang Zhang,Xixi Shen,Wei Wang

Chinese chicken broth is well known for its outstanding nutritional value and flavor, widely consumed in China. This study was designed to develop a sensitive and accurate high-performance liquid chromatography-variable wavelength detector (HPLC-VWD) method to simultaneously determine purines and uric acid in Chinese chicken broth for gout and hyperuricemia dietary management. Chromatographic separation was performed on an Agilent TC-C18 (2) column (4.6 mm × 250 mm, 5.0 µm), using 0.02 M KH2PO4(pH 4.0) as a mobile phase. Sample pretreatment was optimized to enable the extraction of all analytes from Chinese chicken broth. The optimal pretreatment conditions were chicken broth-60% trifluoroacetic acid (TFA)/20% formic acid (FA) (1:1,v/v) in a volume ratio of 1:3 and hydrolysis for 40 min at 85 °C in a water bath. The limits of detection (LODs) and limits of quantification (LOQs) of the purines and uric acid were 0.58–1.71 µg/L and 1.92–5.70 µg/L, respectively. The recoveries were 91–101%, with the relative standard deviations (RSDs) lower than 3%. The complete method has been successfully applied to determine purines and uric acid in various Chinese chicken soups obtained from different provinces in China.Keywords:Chinese chicken broth;purine;uric acid;HPLC;acid hydrolysis;hyperuricemia;gout

CAS / MDL: 64-18-6 76-05-1
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Food Chemistry-X · 2023 · IF 6.1

A screening for optimal selenium enrichment additives for selenium-enriched fish production: Application of a HPLC-ICP-MS method

Chao Zhu,Qimin Liu,Yang Wang,Xiaolin Wang,Yuxuan Ma,Fangxia Yang,Wuzi Dong,Hong Ji

The production of selenium-enriched fish contributes to alleviating selenium deficiency for humans. In this study, selenium nanoparticles (SeNPs) comparable in bioavailability to selenomethionine (SeMet), increased SeMet content in O. macrolepis ( Onychostoma macrolepis ) muscle. Additionally, dietary SeNPs significantly enhanced selenocysteine (SeCys 2 ) and methylselenocysteine (MeSeCys) levels in O. macrolepis muscle. The effect of SeNPs on selenium speciation in grass carp muscle was consistent with O. macrolepis results. SeCys 2 and MeSeCys showed antioxidant capacity in HEK293T cells, indicating enhanced health benefits of Se-enriched fish produced using SeNPs. Furthermore, the addition of 0.3 mg/kg SeNPs significantly improved the flesh quality of O. macrolepis by reducing the content of crude fat and heavy metals, as well as increasing the levels of crude protein, eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), and the ratio of n-3/n-6 polyunsaturated fatty acids (PUFAs). Therefore, selenium-enriched fish produced from SeNPs is a good source for improving human dietary selenium intake.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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MICROCHEMICAL JOURNAL · 2026 · IF 5.2

Residue accumulation-guided preparation of grass carp matrix candidate reference materials for four nitrofuran metabolites using HPLC-MS/MS

Chaoying Zhang,Bohao Qi,Xin Huang,Jincheng Li,Yingchun Mu,Huan Liu

A residue accumulation-guided strategy was developed for preparing grass carp matrix candidate reference materials. • Parent nitrofuran drugs were introduced by medicated bath to generate four marker metabolites in fish muscle. • HPLC–MS/MS enabled reliable quantification of nitrofuran marker metabolites in grass carp powder. • A 10 h bath exposure at 25 °C achieved target residue levels of 5–10 μg/kg. • The prepared candidate materials showed acceptable homogeneity, stability, and batch-to-batch reproducibility. The preparation of incurred aquatic matrix candidate reference materials remains challenging because residue formation is influenced by biological exposure processes and matrix interactions. In this study, a residue accumulation-guided strategy was developed for the preparation of a grass carp matrix candidate reference material containing four nitrofuran marker metabolites, including semicarbazide (SEM), 3-amino-2-oxazolidinone (AOZ), 1-aminohydantoin (AHD), and 3-amino-5-morpholinomethyl-2-oxazolidinone (AMOZ). The relationship between medicated-bath exposure conditions and muscle residue levels was evaluated and used to determine practical preparation conditions. Under the optimized exposure conditions, grass carp samples were collected, homogenized, freeze-dried, ground, sieved, and blended to obtain a homogeneous candidate material. The prepared candidate material showed acceptable homogeneity and stability under the investigated conditions and yielded batch-to-batch reproducibility with RSD values of 1.9–3.2% for 0.4 g freeze-dried test portions. The developed material exhibited suitable characteristics for potential applications in analytical quality assurance, method comparison, and related scientific studies. This study provides an alternative strategy for preparing grass carp matrix candidate reference materials containing incurred nitrofuran marker metabolites through controlled biological exposure and residue accumulation-guided preparation. Download: Download high-res image (172KB) Download: Download full-size image

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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2023 · IF 3

Simultaneous quantification of donafenib, sorafenib, and their N-oxide metabolites in rat plasma using a HPLC-MS/MS method

Yutao Lou,Zhiyong Sun,Yitao Chai,Hui Qin,Qing Hu,Yujia Liu,Xiaowei Zheng,Ying Hu,Meihua Bao,Jinping Gu,Yiwen Zhang

Donafenib and sorafenib are small molecule chemotherapy drugs for the management of hepatocellular carcinoma, with donafenib being a deuterated derivative of sorafenib. To date, a high liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method that quantify donafenib, sorafenib, and their main metabolites has not yet been developed. The objective of this study was to establish a HPLC-MS/MS method for the simultaneous detection of donafenib, donafenib-N-oxide, sorafenib, and sorafenib-N-oxide and for the pharmacokinetic studies in rat. The extraction of all analytes was achieved by simple protein precipitation utilizing acetonitrile. The Waters XBridge C 18 column (2.1 × 100 mm, 3.5 µm) was selected, and the analytes could be efficiently separated and quantitated during a 2.8 min gradient elution procedure. The method was linear within the predefined quantification ranges and provided acceptable precision (%CV < 9.4%), reproducible extraction recovery (99.4%–111.5%), and low matrix effect (88.1%–98.6%). The hemolysis effect did not interfere with the quantification of all analytes, and similar results were obtained by changing the anticoagulant K 2 -EDTA to heparin or sodium citrate. Plasma pharmacokinetics revealed that the values of t 1/2 , C max , and AUC 0-t of donafenib were 1.4-, 6.2-, and 3.1-fold higher than those of sorafenib, respectively. In conclusion, the proposed bioassay was successfully applied to pharmacokinetic studies in rat after administration of donafenib and sorafenib. Our work not only improves the bioanalytical method for determining the plasma concentrations of donafenib, sorafenib, and their N-oxide metabolites, but also provides a scientific reference for clinical pharmacokinetic studies.

✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2023 · IF 3

Improved liquid-liquid extraction followed by HPLC-UV for accurate and eco-friendly determination of tetramethylpyrazine in vinegar products

Hong Yang,Jing Wang,Wenming Cao

Tetramethylpyrazine (TMP) is an important bioactive compound in vinegars, contributing to their health-enhancing attributes. It serves as a crucial benchmark for the assessment of vinegar quality. Unfortunately, inaccuracies have arisen due to incomplete extraction techniques and the use of an inappropriate standard substance. These challenges have significantly curtailed comprehensive exploration into the underlying TMP formation mechanisms, impeding advancements within prevailing benchmarks and methodologies governing vinegar products. To address these challenges, several critical parameters, encompassing pH, solvent type, centrifugal force, extraction times and reference materials were investigated and optimized. The TMP content was determined by adjusting the pH to 9 using a sodium hydroxide solution, followed by extraction with ethyl acetate and subsequent re-extraction of the ethyl acetate layer with 0.2 mol/L HCl. A high-performance liquid chromatography method with an ultraviolet detector (UV) was developed and validated. This method demonstrated superior sensitivity compared to existing methods, with a limit of detection (LOD) of 0.0237 μg/g, limit of quantification (LOQ) of 0.0829 μg/g, method limit of detection (MLOD) of 0.10 μg/g and method limit of quantitation (MLOQ) of 0.25 μg/g. The modified method exhibited excellent linearity for TMP in the range of 0.1–118.4 μg/mL, with a good correlation coefficient (R 2  > 0.999). The recovery rate of TMP in vinegar products ranged from 82.4 to 96.2%. Consequently, the proposed method exhibits substantial promise for systematic inquiry into TMP formation mechanisms and for ensuring consistent quality control during the production of premium-grade vinegars.

CAS / MDL: 1124-11-4
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LWT-FOOD SCIENCE AND TECHNOLOGY · 2023 · IF 6

Characterization of anthocyanins in Gynura bicolor DC using HPLC-Q-Orbitrap MS and its stability during microwave vacuum drying

Zhenbao Jia,Hua Liu,Wenwei Chen,Fei Tao

Gynura bicolor DC ( G. bicolor ) is largely consumed as a vegetable in many parts of the world, and due to its content in anthocyanin can be considered as a health-promoting food. This study aimed to characterize the anthocyanin composition of G. bicolor and compare the effect of microwave vacuum drying (MVD) on the anthocyanin content with that of hot air drying (HAD). Anthocyanins were characterized using high-performance liquid chromatography-quadrupole-Orbitrap mass spectrometry (HPLC-Q-Orbitrap MS), which accurately identified five anthocyanin compounds. Delphinidin 3- O -neohesperidoside is the main anthocyanin compound found in G. bicolor . MVD decreased the drying time by 89% compared to HAD. MVD retained 87% of the total anthocyanins in G. bicolor , compared to 18% retained by HAD. This study revealed that MVD produced high-quality dried G. bicolor products, while exhibiting reduced processing times compared to those achieved using HAD.

CAS / MDL: 75-05-8 64-18-6 67-56-1
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Food Analytical Methods · 2021 ·Vol. 14 ·期 11 ·2375-2385 · IF 3.366

Magnetic Solid-Phase Extraction Followed by HPLC–DAD for Highly Sensitive Determination of Phthalate Esters in Edible Vegetable Oils

Zhao Yuanli,Zhu Zhenbao,Liu Jianghua,Liu Jichao,Li Guoliang

Phthalate esters (PAEs) are prone to migrate from the plastic containers into oil during production and storage process. Owing to the trace amount of PAEs and complex sample matrix, it is of great importance to explore a facile and sensitive way to extract and detect PAEs from oil samples. In this work, magnetic covalent organic framework nanospheres (Fe 3 O 4 @COF(TbBD)) were fabricated by the aldehyde-amine condensation between benzidine (BD) and 1,3,5-triformylbenzene (Tb) on the surface of Fe 3 O 4 nanoparticles with the help of ultrasonic treatment. The new type nanomaterials were firstly used to the magnetic solid-phase extraction (MSPE) of seven PAEs in edible vegetable oils prior to high performance liquid chromatography coupled with a diode array detector (HPLC–DAD). In order to achieve the best extraction efficiency, several key parameters were optimized. Under optimal conditions, the proposed Fe 3 O 4 @COF(TbBD)-MSPE-HPLC–DAD method possessed high sensitivity (0.55–0.95 µg/kg for LODs and 1.80–3.10 µg/kg for LOQs), good linearity ( R 2  ≥ 0.9983), and satisfactory recoveries (80.2–102.9%). The RSDs for intra-day was less than 6.1%, and inter-day was less than 7.9%. This work not only proposed a rapid and reliable approach for determining PAEs in edible vegetable oils but also broadened the application of magnetic COFs in food determination.

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