Journal of Analytical Methods in Chemistry
·
2025
·Vol. 2025
·期 1
·8995925
·
IF 2.2
Zejun Wang,Qingcheng Wang,Fei Xu,Linhua Wang,Jingjing Liang,Qing Shen,Shunyuan Guo
This study developed a method for simultaneously detecting 10 mycotoxins in Dendrobium officinale using the QuEChERS technique combined with ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS). The method was optimized for sample purification, pretreatment, chromatographic conditions, and mass spectrometric settings. It effectively addressed the matrix effects from impurities like pigments and cellulose. The validation of the method showed good linearity ( R 2 > 0.990), with limits of detection (LODs) ranging from 0.23 to 8.61 μg kg −1 and limits of quantification (LOQs) from 0.77 to 28.7 μg kg −1 . Average recoveries for the 10 mycotoxins ranged from 77.9% to 98.5%, with relative standard deviations (RSD) between 2.26% and 8.28%. The method demonstrated high accuracy, precision, and suitability for large-scale screening of mycotoxins in Dendrobium officinale. When applied to 84 samples, the contamination rate was 2.38%, with the main contaminants being AFB1, ZEN, and AFG1. This method provides a reliable, cost-effective approach for detecting mycotoxin contamination in traditional Chinese medicine.
研究领域:
分析化学
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中药学
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食品安全
·
药物质量控制
·
代谢组学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 39
·期 12
·e70245
·
IF 1.7
Shulu Zhang,Enlin Zhu,Zhibin Wang,Shuang Jiang,Xiaotian Wu,Li Zhang,Xuepeng Shi,Lin Wei,Yuanqiu Mu,Zheng Feng,Yinze Zhong,Xinhui Huang,Yeqing Xu,Chunjuan Yang,Chunli Gan
Syringa oblata Lindl. leaf extract has a long history of use with pharmacological properties such as heat-clearing, detoxifying, and anti-inflammatory effects. In this study, an ulcerative colitis (UC) animal model was established and compared with a normal group. The study simultaneously determined 6 components of S. oblata Lindl. leaf extract (protocatechuic acid, caffeic acid, quercetin 3-O-β-D-glucopyranoside, (8E)-ligstroside, oleuropein, and oleacein) in the plasma of rats. The results showed that the extract exhibited good biological utilization in both groups, with stable metabolism of the six components, maintaining effective plasma concentrations. Pharmacokinetic analysis suggested the extract's potential for UC treatment. The relative standard deviation (RSD) of precision and accuracy for the six components was below 13%, and the lower limits of quantification (LLOQ) were 5.10, 5.10, 10.2, 10.1, 3.39, and 3.18 ng/mL, respectively. The method met FDA bioanalytical validation criteria for stability, matrix effects, and extraction recovery. Significant pharmacokinetic differences between UC and normal rats were observed, highlighting the extract's potential for clinical application and health product development, offering a promising therapeutic option for UC.
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PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2020
·Vol. 43
·期 12
·2290-2300
·
IF 2.878
Guanghui Ren,Huili Chen,Mei Zhang,Nan Yang,Hui Yang,Chuanru Xu,Jiaming Li,Chen Ning,Zhongjin Song,Shiyu Zhou,Siliang Zhang,Xiaoqian Wang,Yang Lu,Ning Li,Yongjie Zhang,Xijing Chen,Di Zhao
Oroxylin A, obtained from the root of Scutellaria baicalensis Georgi , is a flavonoid with antitumor and other pharmacological activities. Our previous studies showed for the first time that it is mainly metabolized to oroxylin A sodium sulfonate by sulfotransferase enzymes in beagle dogs. In this study, rapid, universal, selective, and robust ultra-high-performance liquid chromatography–tandem mass spectrometry methods were established and fully validated to quantitatively detect oroxylin A, oroxylin A 7-O-glucuronide, and oroxylin A sodium sulfonate in beagle dog plasma. The quantitative analysis for oroxylin A sodium sulfonate was reported for the first time. Plasma samples were processed with acetonitrile, a universal protein precipitant. Gradient elution was performed to resolve carryover effects and to achieve separation efficiency and sufficient chromatographic retention. The linear relationships of oroxylin A, oroxylin A 7-O-glucuronide, and oroxylin A sodium sulfonate in plasma were in the range of 2.0–500.0, 5.0–500.0, and 1.881–940.5 ng/mL, respectively. The assay method was successfully applied to pharmacokinetic study. This is the first paper that reveals the pharmacokinetic profile of oroxylin A, oroxylin A 7-O-glucuronide, and oroxylin A sodium sulfonate after single-dose intravenous and oral administration of Oroxylin A in beagle dogs.
研究领域:
药物分析
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药理学
·
代谢组学
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产品关联
DOI
PubMed
高影响因子
Journal of Chemistry
·
2023
·
IF 3
Yan Li,Yuqing Wang,Zhiqiang Zhao,Yunxia Li,Cheng Peng,Jianming Wu
A preliminary study has shown that 3, 8-Di-O-methylellagic acid 2-O-glucoside (DMAG), an ellagic tannin from Sanguisorba officinalis L., has the potential in relieving thrombocytopenia. However, there is a lack of information on the pharmacokinetics of DMAG in thrombocytopenia rats. Therefore, we aimed to establish a simple, rapid, and sensitive UHPLC-MS/MS method for quantifying DMAG and study its pharmacokinetic behavior in this study. DMAG and hispidulin (internal standard, IS) were separated on an Acquity Shim-pack GIST column using 0.1% formic acid in water and acetonitrile as the mobile phase with a total run time of 5 min and gradient elution at a flow rate of 0.3 mL/min. The recovery and matrix effects of DMAG were within 94.85%–100.40% and 94.55%–102.46%, respectively. The intraday RSD and interday RSD were between 3.31% and 13.19%, accuracy RE was ≤6.69%, and stability RSD changes were 3.38%–8.78%. As for intragastric administration, with shortened Tmax (3.00 vs. 2.16 h), Cmax (25.67 vs. 35.38 ng/mL) was added for a 2 mg/kg dose after the establishment of the thrombocytopenia rat model. Relative to normal rats treated with 4 mg/kg, in thrombocytopenia rats treated with the same dose, Cmax (49.13 vs. 67.78 ng/mL), AUC(0–t) (234.60 vs. 318.17 ng·h/mL), and AUC(0–∞) (322.74 vs. 498.57 ng h/mL) increased, MRT (18.15 vs. 26.32 h) prolonged, Tmax (3.00 vs. 2.33 h) shortened, and CL/F (12746.50 vs. 8093.50 mL/h/kg) reduced. As for intravenous administration, Cmax (1679.54 ng/mL), AUC(0–t) (589.02 g·h/mL), and AUC(0–∞) (605.58 g·h/mL) were significantly increased in thrombocytopenia rats than that in normal rats (743.76 ng/mL for Cmax, 242.46 g·h/mL for AUC(0–t), and 245.19 g·h/mL for AUC(0–∞)). Vz/F and CL/F were remarkably decreased from 343196.86 to 194659.43 mL/kg for Vz/F and 8236.18 to 3326.01 mL/h/kg for CL/F with the model establishment, respectively. Overall, we successfully developed a reliable UHPLC-MS/MS method for determining DMAG levels in rat plasma. The pharmacokinetic difference could be attributed to the pathological state of the thrombocytopenia rats, which may affect the absorption, distribution, metabolism, and excretion of DMAG. These findings lay the foundation for further evaluating the clinical efficiency and safety of DMAG in the treatment of thrombocytopenia.
研究领域:
药理学
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分析化学
·
临床医学
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DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2024
·
IF 3.8
Xiao-Fan Lu,Zi-Xuan Nan,Xin-Yu Li,Mei Zhao,Jian-Ping Ma,Wenhua Ji,Dian-Shun Guo
The precise determination of polypeptide antibiotics (PPTs) in foods has been always challenging because of the interference of various endogenous peptides in complex matrix. Herin, a novel large-pore covalent organic framework (TABPT-SPDA-COF) with accessible pore size of 7.9 nm was synthesized as a solid phase extraction (SPE) absorbent for efficiently enriching four PPTs existed in foods originating from animals. The parameters of SPE process were systematically optimized. Subsequently, four PPTs were determined by UHPLC-MS/MS. Under the optimal conditions, TABPT-SPDA-COF shows outstanding enrichment capacity for PPTs in contrast to commercial absorbents ascribed to size selectivity and multiple interaction effects. The method exhibits excellent linear range (0.005–100 ng mL −1 ), satisfactory limits of detection (0.1 pg mL –1 ) as well as relative recoveries (86.2–116 %). This work offers a practicable platform to monitor trace PPTs from complex animal-derived foodstuffs.
研究领域:
分析化学
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食品科学
·
药物分析
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF HAZARDOUS MATERIALS
·
2023
·
IF 13.6
Zenghui Xie,Yuling Hu,Jiana Lin,Gongke Li,Qisheng Zhong
Long-term ingestion or exposure to food contaminated with per- and polyfluoroalkyl substances (PFASs) may cause potential harm to human health. Due to the low contents of PFASs in complex food matrices, it is of great significance to develop adsorbents with excellent properties to enrich PFASs before analysis. Herein, calix[4]arene (CX4) was used as building block to prepare ordered crystalline covalent organic frameworks (COFs). The perfect combination of the host-guest recognition ability of CX4 and the porosity of COFs makes the CX4-COFs selective and high adsorption capacity for linear molecular PFASs (261–1055 mg/g). The adsorption behavior and mechanism were verified by isotherm adsorption experiments and simulation calculations. The CX4-COFs were then used as adsorbents for membrane solid-phase extraction (M-SPE), combined with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) to determine PFASs in food. The method has low detection limits (0.11–0.28 ng/kg) and good precision (1.3%−9.8%), and has been successfully applied to the simultaneous enrichment and determination of six PFASs in fish, shrimp and shellfish. Satisfactory recoveries (79.9%−118%) were obtained. This study provides a new strategy for preparing CX4-COFs containing macrocyclic molecules with different morphologies and expands the application of COFs as attractive enrichment media for sample pretreatment .
研究领域:
食品科学
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环境科学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2023
·
IF 4.8
Zafar Iqbal Tanveer,Qingwen Huang,Tengfei Xu,Yong Chen,Xuesong Liu,Zheng Han,Yongjiang Wu
Fungal species capable of producing aflatoxins frequently contaminate the feed provided to dairy animals, leading to the subsequent occurrence of aflatoxin contamination in milk. Milk is renowned for its exceptional nutritional composition, and the consumption of milk contaminated with aflatoxins by humans can engender a multitude of health complications. In this study, reduced graphene oxide zinc iron oxide ( rGO-Zn/Fe 2 O 4 ) nanomaterial was utilized as a dispersive solid phase extraction adsorbent to separate and enrich aflatoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, and aflatoxin M1) from milk. The rGO-Zn/Fe 2 O 4 nanomaterial was morphologically characterized by scanning electron microscopy, transmission electron microscopy, and X-ray diffraction, indicating that Zn/Fe 2 O 4 nanoparticles were embedded on the surface of rGO. The acetonitrile/formic acid (99/1, v/v) combined with ultrasonic treatment for a duration of 40 min expressed an efficient extraction solvent. Employing the matrix-spiked technique, different parameters of the dispersive solid-phase extraction (d-SPE) method were meticulously optimized, yielding the following conditions: 2% acetonitrile as loading solvent, 15 mg of rGO-Zn/Fe 2 O 4 as the adsorbent quantity, 15 min of ultrasonication as adsorption time, and n-hexane as the washing solvent. The desorption reagent was 5 mL acetonitrile, with a desorption time of 5 min. The combination of the dispersive solid-phase extraction (d-SPE) technique with validated UHPLC-MS/MS quantitative analysis demonstrated excellent selectivity, a robust linear relationship (R 2 ≥ 0.994), remarkable sensitivity (limit of quantification ranging from 0.006 to 0.013 µg/L), and satisfactory recovery rates of 78%–104% at three different matrix-spiked levels. Moreover, the method exhibited precision with relative standard deviations (RSD) ranging from 2.4% to 10.8%. Following appropriate pretreatment procedures, the milk samples underwent rigorous aflatoxin analysis, leading to the identification of AFM1 presence in all of the examined milk samples (n = 9). However, the contamination levels detected were found to be within the permissible limits as defined by regulatory standards.
研究领域:
分析化学
·
食品科学
·
纳米技术
·
毒理学
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产品关联
DOI
高影响因子
MICROCHIMICA ACTA
·
2019
·Vol. 186
·期 12
·1-8
·
IF 5.479
Yi Xiaotong,Liu Chang,Liu Xueke,Wang Peng,Zhou Zhiqiang,Liu Donghui
Magnetic partially carbonized cellulose nanocrystals (MPC-CNC) were obtained by sulfuric acid treatment of microcrystalline cellulose (MCC) and then loaded with magnetic Fe 3 O 4 nanoparticles. The material is shown to be a viable material for magnetic solid phase extraction of triazine and triazole pesticides from water. The pesticides (specifically: simazine, ametryn, prometryn, terbutryn, atrazine, triadimenol, epoxiconazole, myclobutanil, triadimefon and tebuconazole) were quantified by ultra HPLC in tandem with a triple quadrupole mass spectrometry (UHPLC-MS/MS). The effects of NaCl concentration, amount of adsorbent, vortex time, sample volume and pH value on extraction efficiency were optimized by Plackett-Burman design and Box-Behnken design methods. Under the optimal conditions, the method shows the following figures of merit: (a) Linear responses in the range from 0.02–10 μg L −1 ; (b) detection limits between 2.2 to 6.1 ng L −1 (for S/ N = 3); (c) recoveries from spiked samples of 73.7–117.1% with relative standard deviations (RSDs) of 2.0–15.7%; and (d) an enrichment factor of 75. The method was successfully applied to the determination of the pesticides in five environmental water samples.
Schematic representation of the process of magnetic solid phase extracting pesticides in water using MPC-CNC. MCC-microcrystalline cellulose; PC-CNC- partially carbonized cellulose nanocrystals; MPC-CNC-magnetic partially carbonized cellulose nanocrystals.
研究领域:
环境科学
·
分析化学
·
纳米技术
·
水质分析
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产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2022
·Vol. 14
·期 22
·2227-2234
·
IF 3.532
Guilin Liu,Yunhai Duan,Shuang Yang,Mingming Yu,Zhihua Lv
A sensitive and robust ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was established for the first time to simultaneously quantify marine neutral neoagaro-oligosaccharides (NAOS) and agar-oligosaccharides (AOS) with different degrees of polymerization (DP) in Hanks' balanced salt solution (HBSS). The separation was achieved on a BEH amide column using a mobile phase of acetonitrile-10 mmol L−1 ammonium acetate (58 : 42, v/v) with an isocratic elution program. The total analysis time was 3.5 min. The mass spectra were acquired in the multiple reaction monitoring (MRM) pattern by using a heated-electrospray ionization (H-ESI) source operating in the positive ionization mode. The linear range was 40–20 000 nmol L−1. The accuracy and precision ranged from 91.5 to 110.0% and 0.9 to 10.4%, respectively. The extraction recovery was consistent and reproducible. The stability was within 90.3–110.8%. The matrix effect, carryover, and dilution integrity were all satisfactory. Moreover, the validated method was successfully applied to the intestinal transport study by using the Caco-2 cell monolayer in vitro. The results revealed that neoagarobiose, neoagarotetraose, neoagarohexaose, agarotriose, agaropentose, and agaroheptose were transported by a paracellular pathway.
研究领域:
分析化学
·
药学
·
生物医学工程
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Guangyi Zhang,Chengqiang Han,Yuxuan Li,Xi-Ling Li,Hongmei Jin,Jun Zhe Min
α-Dicarbonyl compounds (α-DCs) in human saliva are closely associated with diabetes, but their inherent instability presents challenges for sample transportation and detection. This study introduces a novel approach for the simultaneous detection of three α-DCs—3-deoxyglucoside (3-DG), glyoxal (GO), and methylglyoxal (MG)—in dried saliva spots using 4,5-dimethyl-1,2-phenylenediamine (DMPD) derivatization combined with UHPLC-MS/MS. 5.0 mm diameter double-circle qualitative filter paper was selected as the substrate for dried saliva, with optimal extraction conditions involving two 3-minute extractions. Chromatographic separation was performed on a CSH™ C18 column (2.1 × 50 mm, 1.7 μm) via gradient elution, utilizing a mobile phase consisting of 0.1 % formic acid in water and 0.1 % formic acid in acetonitrile. The entire separation process was completed within a 5.0 min timeframe. The linearity of 3-DG and GO in the concentration range of 0.10–12.5 μM, and MG in the range of 0.24–31.25 μM. (R 2 ≥ 0.9994). Intra- and inter-day precision yielded RSD values ranging from 0.59 % to 5.78 %, with average recoveries between 99.78 % and 108.50 %. The detection limits were 0.85–12.85 fmol. This method was applied to analyze dried saliva samples from 44 healthy volunteers (HVs) and 46 diabetic patients (DPs), revealing significant differences ( p < 0.001) in the concentrations of 3-DG, GO, and MG between HVs and DPs. The research outcomes validate the practicality of α-DCs in dried saliva samples as prospective biomarker candidates for diabetes, while introducing an innovative methodology for their utilization in clinical settings.
研究领域:
分析化学
·
临床化学
·
糖尿病研究
·
代谢组学
·
生物分析方法开发
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产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2025
·
IF 9.8
Wenxiu Zhou,Bingjie Li,Ke Xu,Shengman Zhang,Zhaoqian Li,Xin Wang
The residues of antiviral drugs acyclovir (ACV), penciclovir (PCV) and ganciclovir (GCV) in foods, particularly in ready-to-eat products, pose a significant threat to human health, making it urgent to develop a rapid and sensitive method for their detection. Herein, we designed a novel magnetic molecularly imprinted three-dimensional covalent organic framework (MICOF@Fe 3 O 4 ) for selective extraction of these antiviral drugs from complicated food matrix. The prepared MICOF@Fe 3 O 4 integrates molecular recognition ability, 3D COF structural advantages and magnetic responsiveness, providing high selectivity, large adsorption capacity and facile operation for magnetic solid-phase extraction (MSPE). Afterwards, a MSPE-UHPLC-MS/MS method was developed, which stands out as the most sensitive approach yet for ACV, PCV, GCV measurements and has been successfully applied to analyze thirteen ready-to-eat chicken samples. Endogenous PCV was detected in two of these samples, demonstrating the potential of the proposed method as a valuable tool for monitoring antiviral drug residues and ensuring food safety.
研究领域:
分析化学
·
食品安全
·
材料科学
·
药物分析
·
环境科学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2016
·
IF 3.169
Jian-Ping Li,Jian-Ming Guo,Er-Xin Shang,Zhen-Hua Zhu,Yang Liu,Bu-Chang Zhao,Jing Zhao,Zhi-Shu Tang,Jin-Ao Duan
Acetylsalicylic acid (Aspirin, ASA) is a famous drug for cardiovascular diseases in recent years. Effects of ASA dosage on the metabolic profile have not been fully understood. The purpose of our study is to establish a rapid and reliable method to quantify ASA metabolites in biological matrices, especially for glucuronide metabolites whose standards are not commercially available. Then we applied this method to evaluate the effects of ASA dosage on the metabolic and excretion profile of ASA metabolites in rat urine. Salicylic acid (SA), gentisic acid (GA) and salicyluric acid (SUA) were determined directly by UHPLC–MS/MS, while salicyl phenolic glucuronide (SAPG) and salicyluric acid phenolic glucuronide (SUAPG) were quantified indirectly by measuring the released SA and SUA from SAPG and SUAPG after β-glucuronidase digestion. SUA and SUAPG were the major metabolites of ASA in rat urine 24 h after ASA administration, which accounted for 50% (SUA) and 26% (SUAPG). When ASA dosage was increased, the contributions dropped to 32% and 18%, respectively. The excretion of other three metabolites (GA, SA and SAPG) however showed remarkable increases by 16%, 6% and 4%, respectively. In addition, SUA and SUAPG were mainly excreted in the time period of 12–24 h, while GA was excreted in the earlier time periods (0–4 h and 4–8 h). SA was mainly excreted in the time period of 0–4 h and 12–24 h. And the excretion of SAPG was equally distributed in the four time periods. We went further to show that the excretion of five metabolites in rat urine was delayed when ASA dosage was increased. In conclusion, we have developed a rapid and sensitive method to determine the five ASA metabolites (SA, GA, SUA, SAPG and SUAPG) in rat urine. We showed that ASA dosage could significantly influence the metabolic and excretion profile of ASA metabolites in rat urine.
研究领域:
药理学
·
分析化学
·
代谢组学
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产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）