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MOLECULES · 2022 ·Vol. 27 ·期 21 ·7636 · IF 4.927

Simultaneous Determination of 108 Pesticide Residues in Three Traditional Chinese Medicines Using a Modified QuEChERS Mixed Sample Preparation Method and HPLC-MS/MS

Xuyan Fan,Tao Tang,Song Du,Ningning Sang,Hao Huang,Chenghui Zhang,Xueping Zhao

A rapid, efficient, simple, and high-throughput method for the simultaneous determination of 108 pesticide residues in three traditional Chinese medicines (TCMs) was established, comprising an improved QuEChERS method in combination with HPLC-MS/MS based on mixed samples. A quantity of 10 mL of acetonitrile was used as extraction solvent, and 10 mg of amino-modified multi-walled carbon nanotubes (MWCNTs-NH2) and 150 mg of anhydrous magnesium sulfate (MgSO4) were selected as sorbents for dispersive solid phase extraction. The performance of the method was verified according to the analytical quality control standards of SANTE/11813/2017 guidelines. With good linearity (R2> 0.9984) in the range of 2–200 μg/L for all pesticides in the selected matrices, and good accuracy, precision, and high sensitivity, the recoveries were in the range of 70–120% for more than 95% of the pesticides, with a relative standard deviation (RSD) of less than 16.82% for all. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.01–3.87 μg/kg and 0.07–12.90 μg/kg, respectively, forFritillaria thunbergiiMiq (F. thunbergii),Chrysanthemum MorifoliumRamat (C. morifolium), andDendrobium officinaleKimura et Migo (D. officinale). The method was successfully applied to 60 batches of actual samples from different regions.Keywords:pesticide residue;QuEChERS;MWCNTs-NH2;traditional Chinese medicines

CAS / MDL: 308068-56-6 1314-23-4
研究领域: 分析化学 · 药学
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Current Analytical Chemistry · 2024 ·Vol. 21 ·期 2 ·124-133 · IF 1.7

A Low-cost and Rapid Method for Determination of Five Flavonoids in Herbal Medicines with Rutin by HPLC-UV at Equal Absorption Wavelength

Zhengming Qian,Zhuobin He,Dongyin Lian,Qi Huang,Guoying Tan,Juying Xie

BackgroundFlavonoid is a type of active constituent in herbs and always used as the quality control markers of herbal medicines. Owing to the extensive diversity of flavonoids, numerous reference compounds are necessitated for the analysis of flavonoids, and some are usually very expensive, which engenders challenges in the analysis of flavonoids in herbal medicines. Consequently, the development of a simple, rapid, and reference compounds saving method is important for the determination of flavonoids in herbal medicines.ObjectiveIn order to develop a high-performance liquid chromatography (HPLC) method for the determination of 5 flavonoids (mangiferin, hesperidin, baicalin, buddleoside, and rutin) in five herbal medicines (Anemarrhenae rhizome, Sophorae flos, Citri reticulatae pericarpium, Scutellariae radix, and Chrysanthemi indici flos) with rutin.MethodsFive herbal medicine samples were prepared according to the Chinese Pharmacopoeia which includes ultrasound and reflux methods. The separation of the sample was performed on a PoroShell 120 EC-C18 (4.6 mm×100 mm, 2.7 μm) by gradient elution with 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. The wavelengths were set as follows: Anemarrhenae rhizome (363 nm), Sophorae flos (256 nm), Citri reticulatae pericarpium (236 nm), Scutellariae radix (263 nm), Chrysanthemi indici flos (354 nm).ResultsThe method validation showed that the established HPLC method was accurate and stable for quantitative analysis of flavonoids in five herbal medicines. The comparative analysis revealed that the determination results of the current HPLC method and Chinese Pharmacopoeia method are consistent, exhibiting less than 1% relative error. Remarkably, the developed HPLC method needs one cheapest reference compound (rutin) and costs 8 min for sample HPLC analysis.ConclusionThe developed HPLC method for quantitative analysis of five flavonoids in five herbal medicines is simple, rapid, and reference compound saving, which provides a good alternative method for quality control of flavonoids in herbal medicines.

研究领域: 药学 · 分析化学
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MOLECULES · 2020 ·Vol. 25 ·期 16 ·3749 · IF 3.267

The Potential Transformation Mechanisms of the Marker Components of Schizonepetae Spica and Its Charred Product

Xindan Liu,Ying Zhang,Menghua Wu,Zhiguo Ma,Hui Cao

Schizonepetae Spica (SS) is commonly used for treating colds, fevers, bloody stool and metrorrhagia in China. To treat colds and fevers, traditional Chinese medicine doctors often use raw SS, while to treat bloody stool and metrorrhagia, they usually use Schizonepetae Spica Carbonisata (SSC; raw SS processed by stir-frying until carbonization). However, there have been limited investigations designed to uncover the mechanism of stir-fry processing. In the present study, a method combining gas chromatography-mass spectrometry (GC-MS) and high-performance liquid chromatography (HPLC) was developed for the comprehensive analysis of the chemical profiles of SS and SSC samples. Principal component analysis of the GC-MS data demonstrated that there were 16 significant differences in volatile compounds between the SS and SSC samples. The simultaneous quantification of six nonvolatile compounds was also established based on HPLC, and remarkable differences were found between the two products. These changes were probably responsible for the various pharmacological effects of SS and SSC as well as the observed hepatotoxicity. Finally, the mechanisms could be rationalized by deducing possible reactions involved in the transformation of these marker components. This work reports a new strategy to reveal the chemical transformation of SS during stir-fry processing.Keywords:Chinese medicinal material;Schizonepetae Spica;Schizonepetae Spica Carbonisata;stir-frying;marker component;transformation mechanism

CAS / MDL: 141-78-6
研究领域: 中药学 · 分析化学
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2021 · IF 3.205

Development a multi-immunoaffinity column LC-MS-MS method for comprehensive investigation of mycotoxins contamination and co-occurrence in traditional Chinese medicinal materials

Dan-Tong Zhao,Yi-Jun Gao,Wen-Jin Zhang,Tian-Chen Bi,Xiao Wang,Chun-Xia Ma,Rong Rong

Mycotoxins are poisonous secondary fungal toxic metabolites and harmful to human health. Traditional Chinese medicinal materials (TCMs), including more than two hundred functional foods, are vulnerably bred fungi, causing spoilage and multi-mycotoxins contamination. This study established a simultaneous analytical method by using multi-mycotoxins immunoaffinity column (multi-IAC) and HPLC-MS/MS to evaluate mycotoxins' contamination levels and natural incidence in TCMs. Aflatoxins (AFs, including AFB1, AFB2, AFG1 and AFG2), ochratoxin A (OTA), fumonisins (FB1 and FB2), zearalenone (ZEN), deoxynivalenol (DON) and T-2 toxins in three TCMs or functional foods of Polygalae Radix (PR), Coicis Semen (CS) and Eupolyphaga Steleophaga (ES) were detected. The systematically investigated results of 30 batch AFB1 positive samples revealed co-occurrence and correlation of multi-mycotoxins are significant differences in various matrices. All the samples in this study contain more than 5 mycotoxins. AFB1-AFs, AFB1-FBs, AFB1-DON, and AFB1-T-2 are the most observed co-occurrence, AFB1-OTA is also of concern due to its synergistic toxicity. This study's results can be used to establish guidelines for screening mycotoxin contaminants and limitations on acceptable levels in TCMs. Simultaneously, mycotoxin's correlation results in different matrices can also provide a reference for the standardization of TCM production and processing.

研究领域: 食品科学 · 分析化学 · 毒理学
✓ 已验证 DOI PubMed 高影响因子
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JOURNAL OF SUPERCRITICAL FLUIDS · 2021 · IF 4.577

Modelling of continuous supercritical fluids extraction to recover fatty and volatile oil from Traditional Chinese Medicinal materials

Jia Jingfu,Shi Qinglong,Qing Chengyuan,Zhang yue,Zhou dan,Ge Fahuan

Several classical Chinese herbal materials (CHMs) were extracted using continuous supercritical fluid extraction (CSFE), a newly developed technology to further elevate the efficiency of traditional batch supercritical fluid extraction (SFE). A mathematical model was established to describe CSFE process and predict the optimal switching times. The results showed that the total extraction times of Ganoderma lucidum spores (S- GL ), Juglans regia seeds, Zingiber officinale rhizoma and Citrus reticulata pericarp by CSFE were 55.2%, 40.3%, 55.5% and 36.0% lower than those by batch SFE, respectively. Furthermore, mathematical predictions could further help to improve the extraction efficiency and make full utilization of CHMs. When using the calculated optimal switching times, the total extraction rate of CSFE kept constant at the maximum value. Qualities of CHMs extracts had no significant difference between batch SFE and CSFE. The mathematical model of CSFE can be used to guide the extraction of active ingredients from CHMs.

CAS / MDL: 75-05-8 110-54-3
研究领域: 药学 · 植物化学
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MICROCHEMICAL JOURNAL · 2024 · IF 4.9

Uniform spherical covalent organic framework for efficient extraction of 13 per-and polyfluoroalkyl substances in Chinese medicinal materials

Ziyue Ni,Yiran Zhou,Meng Shan,Ting Gui,Junhong Xin,Yunlun Li

Long-term consumption or exposure to Chinese medicinal materials contaminated with per- and polyfluoroalkyl substances (PFASs) poses a potential risk to human health. Owing to the low contents of PFASs in the complex matrix of Chinese medicinal materials, it is imperative to develop high-performance adsorbents for the enrichment of PFASs prior to analysis. Covalent organic frameworks (COFs) are widely used as adsorbents because of their large surface area and good chemical stability. In this study, C N bonded spherical TPB-DMTP-COF was prepared by a simple Schiff base reaction using acetonitrile as solvent at room temperature. The materials exhibited abundant porous structures, exceptional hydrophobicity, superb thermostability, excellent crystalline structure, and a substantial surface area of 1419 m 2 g −1 and thus could be outstanding adsorbents for solid-phase extraction (SPE) of PFASs. The adsorption experiments showed that the adsorption capacity and adsorption rate of PFASs increased with the extension of alkyl carbon chain of PFASs molecule. In essence, the strong adsorption affinity could be attributed to the hydrophobic characteristics and Van der Waals force. The proposed approach based on SPE and liquid chromatography-tandem mass spectrometry achieved low limits of detection (0.01–0.04 μg kg −1 ), good precision (< 4.7%) and excellent linearity for PFASs ranging from 0.1 to 10 ng mL −1 (R 2  ≥ 0.997). The actual amounts of PFASs varied from 0.08 μg kg −1 to 2.67 μg kg −1 in seven Chinese medicinal materials. The satisfactory recoveries (91.6%–105.8%) and good repeatability (12 times) for simultaneous analysis of 13 PFASs were obtained. This research presents a promising alternative for the sensitive analysis of PFASs at trace levels in complex matrices.

CAS / MDL: 631-61-8 108-67-8
研究领域: 环境科学 · 分析化学 · 药学
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ANALYTICA CHIMICA ACTA · 2017 · IF 4.95

A strategy to identify and quantify closely related adulterant herbal materials by mass spectrometry-based partial least squares regression

Li Wang,Li-Fang Liu,Jian-Ying Wang,Zi-Qi Shi,Wen-Qi Chang,Meng-Lu Chen,Ying-Hao Yin,Yan Jiang,Hui-Jun Li,Ping Li,Zhong-Ping Yao,Gui-Zhong Xin

In this study, a new strategy combining mass spectrometric (MS) techniques with partial least squares regression (PLSR) was proposed to identify and quantify closely related adulterant herbal materials . This strategy involved preparation of adulterated samples, data acquisition and establishment of PLSR model. The approach was accurate, sensitive, durable and universal, and validation of the model was done by detecting the presence of Fritillaria Ussuriensis Bulbus in the adulteration of the bulbs of Fritillaria unibracteata. Herein, three different MS techniques, namely wooden-tip electrospray ionization mass spectrometry (wooden-tip ESI/MS), ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UPLC-QTOF/MS) and UPLC-triple quadrupole tandem mass spectrometry (UPLC-TQ/MS), were applied to obtain MS profiles for establishing PLSR models. All three models afforded good linearity and good accuracy of prediction, with correlation coefficient of prediction ( r p 2 ) of 0.9072, 0.9922 and 0.9904, respectively, and root mean square error of prediction (RMSEP) of 0.1004, 0.0290 and 0.0323, respectively. Thus, this strategy is very promising in tracking the supply chain of herb-based pharmaceutical industry , especially for identifying adulteration of medicinal materials from their closely related herbal species.

研究领域: 药物分析 · 中药质量控制 · 代谢组学 · 分析化学 · 天然药物化学 · 药物鉴定 · 食品与药品安全
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JOURNAL OF DRUG DELIVERY SCIENCE AND TECHNOLOGY · 2023 · IF 5

Molecular encapsulation of bioactive ingredients from Xuefu Zhuyu decoction by cyclodextrin-assisted extraction

Luyao Wang,Wenhui Li,Lulu Ma,Zhe Zheng,Xin Chai,Huijuan Yu,Yuefei Wang

Enhancing the extraction efficiency of the bioactive ingredients from Chinese medicinal material (CMM) is crucial to effective applications in clinical practice. Herein, focusing on Xuefu Zhuyu decoction (XFZYD) as a classical formula with antithrombotic efficacy, we developed an accessible and environment-friendly method via cyclodextrin (CD) for assisting the extraction of chemical components. The employment of CDs significantly enhanced the extraction efficiency of poorly water-soluble components in XFZYD, from which hydroxypropyl- β -CD (HP- β -CD) showed the best extraction efficiency by comparing to α -CD, β -CD, and γ -CD. Six representative ingredients were focused to systematically perform the encapsulation study between HP- β -CD and guest molecule. The satisfactory association constants of HP- β -CD with the tested compounds were determined by implementing phase solubility method and direct fluorescence technique. The inclusion complexes were studied by DSC and SEM to visualize thermal characteristics and surface textures, which were further confirmed by 1 H NMR spectroscopy. Moreover, theoretical calculations indicated that stable bindings between HP- β -CD and tested compounds were witnessed by various non-covalent interactions. Thus, the formation of the inclusion complex with CD is a very effective method to improve the extraction efficiency of the active compounds from CMM.

CAS / MDL: 64-18-6
研究领域: 药学 · 中医药 · 化学
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PHYTOCHEMICAL ANALYSIS · 2021 ·Vol. 33 ·期 3 ·441-451 · IF 3.373

Development of an immunochromatographic test strip for the rapid detection of aristolochic acid A in herbal medicinal materials

Xianrui Chen,Ting Huang,Zhibing Huang,Quanbin Han

Introduction Plants containing aristolochic acid and its derivatives are nephrotoxic, mutagenic, and carcinogenic to humans; chronic diet poisoning caused by the aristolochic acid is the cause of endemic (Balkan) nephropathy and related cancers. Objective To develop a colloidal gold immunochromatographic test strip (ICS) based on the competitive format for the rapid detection of aristolochic acid A (AA-A) in herbal medicinal materials. Materials and methods For the ICS based on gold nanoparticles (AuNPs), the antigen [AA-A–bovine serum albumin (BSA)], and goat anti-mouse IgG were drawn on the nitrocellulose membrane as the test line (T line) and the control line (C line), respectively. Monoclonal antibody (MAb)–AuNP conjugates were sprayed onto the conjugate pad. The sensitivity of the ICS was 6 ng/mL, and the test was completed in 10 min. The analysis of AA-A in traditional Chinese medicine samples showed that the ICS results were in good agreement with those obtained by high-performance liquid chromatography methods. Conclusion These results demonstrated that the ICS test could be used as a reliable, rapid, cost-effective, and convenient qualitative tool for on-site screening techniques to detect AA-A in herbal medicinal materials without any special instrumentation.

研究领域: 药理学 · 分析化学 · 毒理学 · 医学
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