Journal of Ocean University of China
·
2023
·Vol. 22
·期 6
·1683-1691
·
IF 1.6
Yue Jiali,Cheng Wei,Wei Shutong,Liu Guilin,Zhou Meichen,Lv Zhihua,Yu Mingming
A sensitive, rapid, and robust ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was established for the first time to quantify agarotriose (A3) in rat plasma, tissues, urine, and feces. A3 and stachyose (internal standard) were separated by a BEH amide column at 65 °C under the mobile phase of 10 mmol L −1 ammonium acetate-acetonitrile (42:58, v / v ) with 350 µL min −1 . The acquisition of transitions was carried out in multiple reaction monitoring (MRM) pattern operating with positive ionization at m / z 509.16 ≥ 329.15 for A3 and m / z 689.15 ≥ 527.11 for stachyose. The linearity ranges of A3 were 10 to 5000 nmolL −1 for plasma, 20 to 10000 nmolL −1 for tissues, and 40 to 20000 nmolL −1 for urine and feces. The accuracy and precision ranged from 90.9% to 111.6% and 0.7% to 10.1%, respectively. The stability was between 86.1% and 102.5%. The extraction recovery was consistent and reproducible. The matrix effect ranged from 1.5% to 11.4%. The pharmacokinetic, tissue distribution, and excretion studies were successfully conducted with the validated method. Results showed that A3 could be absorbed by rats, and the absolute bioavailability was 6.7%. Furthermore, it was rapidly distributed in rat tissues and mainly eliminated via feces excretion (67.0%) after oral administration. For intravenous bolus, 85.5% was recovered, and renal excretion was the primary pathway (77.6%) for cumulative recovery.
研究领域:
分析化学
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药理学
·
代谢组学
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DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.1
Qing-nan Chen,Yun-e Bai,Yao Ma,Rui Liao,Lu-lu Wang,Shuang Hu,Jian- ping Gao
Latex-bearing plants have gained global attention, but few studies have been reported on Codonopsis pilosula (Franch.) Nannf.( C. pilosula ) latex. In this research, we established a UHPLC-MS/MS method to investigate the constituents in C. pilosula latex. Analysis revealed that the latex of C. pilosula contains alkaloids, terpenoids, and fatty acids, with fatty acids being one of the primary metabolites distinguishing the latex from above-ground (DS) and below-ground (DX) parts of C. pilosula. To evaluate the quality of C. pilosula latex, an approach of dispersive liquid-liquid microextraction with solidification of the floating organic drop (DLLME-SFO) methodology was developed to quantitatively analyze the contents of three fatty acids (palmitic, linoleic, and stearic) in the latex of C. pilosula . The ideal extraction conditions involve injecting 20 μL of dodecanol extractant into a 5 mL 10% NaCl solution at pH 3.0, followed by 20 min at 700 rpm. The three components mentioned above have enrichment coefficients ranging from 48 to 50. The quantification limits were between 0.23 and 0.25 μg/mL, and three components demonstrated good linearity in their respective linear ranges (R 2 > 0.995). The satisfied precision and recovery rates were 1.26 to 8.05% and 92.38 to 101.53%, respectively. By quantitatively analyzing the three fatty acid contents in the latex of C. pilosula , the results showed that palmitic and linoleic acids were able to successfully distinguish the latex of C. pilosula from different parts, which laid the foundation for the quality evaluation of C. pilosula , and provided a reference for the utilization of C. pilosula , a medicinal food source.
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高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2025
·
IF 3.1
Zheming Yu,Yangyang Chen,Fengting Ou,Kui Zeng,Debo He,Lushan Yu
The aim of this study was to develop and fully validate a sensitive and rapid ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneous quantification of Dimyristoyl phosphatidylcholine (DMPC) and Dimyristoyl phosphatidylglycerol (DMPG) in biological matrices of rats after intravenous administration of amphotericin B phospholipid complex suspension injection and excipients (DMPC and DMPG). DMPC, DMPG and Loratadine (internal standard, IS) were separated on an Agilent ZORBAX Extend-C18 column (2.1 mm × 50 mm, 3.5 μm particle size) by using gradient elution consisting of isopropanol-acetonitrile (90:10, v/v, 10 mM ammonium formate and 0.1 % formic acid) and water (10 mM ammonium formate and 0.1 % formic acid) at a flow rate of 0.3 mL/min in 4.0 min. Multiple reaction monitoring (MRM) mode was performed to quantify data under monitoring precursor-product ion transitions of m/z 678.9→184.0 (DMPC, ESI+), 665.5→227.2 (DMPG, ESI-) and 383.0→337.1 (loratadine, IS, ESI+), respectively. The method was developed at linearity ranging from 10.0 to 1000 ng/mL for all analytes. The inter-day accuracy of DMPC and DMPG was observed to range between −12.8–12.7 %, while the precision was found to be within 15.0 %. DMPC and DMPG demonstrated stability during sample storage, preparation and analytic procedures. Furthermore, this method was successfully applied in the investigation of the pharmacokinetic profile and tissue distribution of DMPC and DMPG in rats after intravenous administration. Dose-dependent increases were observed for DMPC and DMPG in both areas under the curve (AUC) and maximum plasma concentration (Cmax), demonstrating positive correlations across all tested dose levels. The biological half-lives (t₁/₂) of DMPC and DMPG following intravenous administration of an amphotericin B phospholipid complex suspension were 1.2–3.4 h and 4.6–8.1 h, respectively. However, after intravenous administration of the excipients, their half-lives were 3.5 h and 1.1–2.3 h. The observed prolongation of DMPC's half-life and concomitant shortening of DMPG's half-life are attributed to the distinct physicochemical properties of the nanoparticles.
研究领域:
药物分析
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药代动力学
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分析化学
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药物递送
·
纳米医学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICAL CHEMISTRY
·
2013
·
IF 5.695
Ruichuan Yin,Shengquan Liu,Chao Zhao,Meiling Lu,Moon-shong Tang,Hailin Wang
Acrolein (Acr), a ubiquitous environmental pollutant, can react directly with genomic DNA to form mutagenic adducts without undergoing metabolic activation. To sensitively and accurately quantify Acr–DNA adducts (including structural isomers and stereoisomers) in human leukocytes, we developed an enhanced stable isotope dilution ultrahigh performance liquid chromatography (UHPLC)–tandem mass spectrometry (MS/MS) method using ammonium bicarbonate (NH4HCO3), which is thermally unstable and degrades readily to carbon dioxide and ammonia in heated gas phase. Interestingly, ammonium bicarbonate (as an additive to the mobile phase) not only improves the protonation of AcrdG adducts but also suppresses the formation of MS signal-deteriorating metal–AcrdG complexes during electrospray ionization, leading to the enhancement of their MS detection by 2.3–8.7 times. In contrast, routinely used ammonium salts (ammonium acetate and ammonium formate) and formic acid do not show similar enhancement. The developed method is potentially useful for enhancing ESI-MS detection of other modified 2′-deoxyribonucleosides that have difficulty in protonation and may form excess metal complexes during electrospray ionization. The limits of detection (LODs, S/N = 3) are estimated to be about 40–80 amol. By the use of the developed method, we found that the Acr adducts of three nucleotides (dG, dA, and dC) can be detected in human leukocytes. In addition to the known γ-AcrdG, α-AcrdA is also identified as an Acr-adduct of high abundance (2.5–20 adducts per108 nts).
研究领域:
分析化学
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环境科学
·
分子生物学
·
毒理学
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DOI
PubMed
高影响因子
Frontiers in Chemistry
·
2022
·
IF 5.545
Zhang Qiaoxuan,Zhan Min,Wu Huihui,Feng Pinning,Jin Xing,Wan Zemin,Yan Jun,Zhang Pengwei,Ke Peifeng,Zhuang Junhua,Zhou Jiuyao,Han Liqiao,Huang Xianzhang
Accurate investigation of adrenal hormone levels plays a vital role in pediatric endocrinology for the detection of steroid-related disorders. This study aims to develop a straightforward, sensitive UHPLC-MS/MS method to quantify 17 endogenous adrenal corticosteroid hormones in human plasma. These hormones are the main ingredients in the synthetic and metabolic pathways of adrenal corticosteroid hormones. Chromatographic separation was achieved on a C18 column before electrospray ionization triple-quadrupole mass spectrometry in multiple reaction monitoring mode with a run time of 7 min. The samples were extracted by liquid-liquid extraction and required no derivatization. Analytical performance was evaluated, including linearity, analytical sensitivity, accuracy, precision, and specificity. Plasma specimens from 32 congenital adrenal hyperplasia (CAH) patients and 30 healthy volunteers were analyzed to further reveal the diagnostic value of multiple steroid hormones in the synthetic and metabolic pathways of adrenal corticosteroid in CAH diagnosis. All hormones were effectively extracted and separated using our method. The method was essentially free from potential interference of isomers or structural analogues. The imprecisions were <10%. The lower limits of quantification varied from 0.05 to 15.0 ng/ml. Good linearity coefficients (r2 > 0.998) were also obtained for most hormones in the required concentration range, except for 21-deoxycortisol (r2 = 0.9967) and androstenediol (r2 = 0.9952). The recoveries for the steroid hormones ranged from 91.7 to 109.8%. We developed the UHPLC-MS/MS method for the simultaneous measurement of steroid hormones. The results showed that measurement of steroid hormones simultaneously could improve the diagnostic efficiency of CAH.
研究领域:
儿科内分泌学
·
临床化学
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DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
Jing Zhou,Hongyu Ning,Haixing Wang,Sen Zhao,Yu Xu,Yilei Fan,Zhongping Huang,Jianhong Gao
Cannabis is the most frequently abused drug worldwide, and the number of cannabis users is still growing. The high lipophilicity of cannabinoids results in extremely low concentrations in wastewater, which poses difficulties and challenges for monitoring cannabinoids. In this study, a hyperbranched mixed-mode anion exchange magnetic adsorbent Fe 3 O 4 @poly(GMA/DVB-WAX) was designed based on the structural characteristics of cannabinoids, which was prepared through copolymerization of glycidyl methacrylate (GMA) and divinylbenzene (DVB) on the surface of oleic acid coated Fe 3 O 4 microspheres followed by hyperbranched modification with ethylenediamine (EDA) and 1,4-butanediol glycidyl ether (BDDGE). This magnetic solid-phase extraction (MSPE) adsorbent can selectively extract four cannabinoids, Δ 9 -tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN), 11-nor-9-carboxy-Δ 9 -tetrahydrocannabinol (THC-COOH), from wastewater through the synergistic effects of hydrophobic interactions, electrostatic interactions, π-π stacking interactions, and hydrogen bonding interactions. The entire extraction time of the adsorbent only takes five minutes and the extraction recovery rates were in the range of 69.4 %-94.0 % for four cannabinoids after the MSPE procedure optimization. An MSPE-UHPLC-MS/MS quantitative method for determination of four cannabinoids in wastewater was established and validated. The results showed that this method had a good linearity within the range of 0.5–100 ng/L (r 2 > 0.9962). The limits of detection and the limits of quantification were 0.17–0.33 ng/L and 0.50–1.00 ng/L, respectively. The proposed MSPE-UHPLC-MS/MS method based on Fe 3 O 4 @poly(GMA/DVB-WAX) is a convenient, sensitive and reliable strategy and has great application prospects in the analysis of trace cannabinoids in wastewater.
研究领域:
分析化学
·
环境科学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 4
·775
·
IF 4.2
Liyuan Ma,Qiaoling Yu,Meng Zhuang,Chen Yang,Yuan Liu,Yuling Li,Cheng Liu,Xiaoyan Shen,Yan Chang
Legubicin, a novel prodrug based on doxorubicin, has both albumin-binding and legumain-activating properties. The aim of this study was to develop and validate a UHPLC-MS/MS method for investigating the in vivo pharmacokinetics and tissue distribution profiles of legubicin in rats and tumor-bearing mice following intravenous administration, and to compare this prodrug with the positive control drug doxorubicin. The study employed a UHLC-MS/MS method to determine the levels of albumin-bound of legubicin and two metabolites (free Leu-DOX and DOX) in plasma, tumor, and tissue samples. This method was validated for good selectivity, high sensitivity, excellent extraction recovery, and short run time. The results showed that legubicin was present in the circulation in vivo mainly in a protein-bound form with larger AUC values and lower clearance and distribution, and essentially released small amounts of doxorubicin. Compared to administration of equimolar doses of doxorubicin, legubicin showed increased exposure of the active drug in the tumor and decreased the level of the active drug in the heart and kidney. This study provides valuable information on the pharmacokinetics and tissue distribution of legubicin, implicating its potential as a novel and effective drug candidate for anti-cancer therapies.
研究领域:
药物化学
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肿瘤学
·
分析化学
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产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2025
·
IF 2.8
Yinshuo Xu,Yuanjie Shan,Yuta Nishio,Kenichiro Todoroki,Toshimasa Toyo'oka,Toufeng Jin,Jun Zhe Min
With the development of untargeted metabolomics, studies have shown that alterations in the serum levels of specific amino acids are strongly correlated with the development of early-stage colorectal cancer (CRC). However, the relationship between optically active free amino acids in human nails and the risk of CRC remains unclear. In this study, a highly sensitive UHPLC-MS/MS chiral separation method based on ( S )-(−)-DBD-Pro-COCl derivatization was established for the simultaneous detection of DL-Asp, DL-Kyn, DL-α-hydroxybutyric acid (DL-α-HB), and Cystamine in the fingernails of patients with CRC. The derivatization reagents were incubated with DL-amino acids, DL-α-HB and Cyst at 60 °C for 15 min to form diastereomers. Subsequently, an Imtakt cadenza CD-C 18 column (3.0 × 150 mm, 3.0 μm) was used for the separation of diastereomers under gradient elution of 10 mM HCOONH 4 in H 2 O as mobile phase A and 0.1 % HCOOH in CH 3 CN as mobile phase B. The degrees of separation (Rs) ranged from 1.76 to 3.21. R 2 was >0.9995, indicating good linearity; the limit of detection (LOD) was 25–100 fmol; the interday and intraday precision of DL-Asp and DL-α-HB detection were 0.85 %–4.91 %; and the average recovery ranged from 81.12 % to 110.2 %. However, during the determination process of fingernail samples, only DL-Asp and DL-α-HB were successfully detected, while DL-Kyn and Cyst were not detected. Therefore, this novel method was used to quantify DL-Asp and DL-α-HB in fingernail samples from 32 healthy volunteers (HVs) and 16 patients with CRC (CPs). The results revealed significant differences in D-Asp ( p < 0.05), L-Asp ( p < 0.01), and L-α-HB ( p < 0.05) levels between male HVs and CPs and in D-α-HB ( p < 0.05) levels between female HVs and CPs. In addition, the D/L-α-HB ratio ( p < 0.01) was significantly different between male HVs and CPs. These findings validate the use of DL-amino acids, DL-α-HB and Cyst from human fingernails as potential diagnostic biomarkers for CRC, providing a basis for the clinical application of human fingernail samples for the noninvasive diagnosis of CRC.
研究领域:
分析化学
·
癌症研究
·
代谢组学
·
临床诊断
·
手性分离
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DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2025
·
IF 3.8
Yu Luyao,Liu Meichen,Niu Ziyi,Zhang Jiarui,Deng Yue,Zhou Xinyue,You Jiansong,Xue Hongyu,Yin Lei,Shi Meiyun
Monodisperse polyethylene glycol (PEG) derivatives offer significant advantages over conventional polydisperse PEGs for biomedical applications due to their precisely defined molecular structures. This study establishes an eco-efficient, selective, and sensitive analytical assay integrating microscale solid-phase extraction (μ-SPE) with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to investigate the cellular uptake of HO-PEG 8 -OH polymers in MCF-7 cells. The method achieved greater than 91% recovery from 20 μL lysates using M-PEG 6 -OH as the internal standard, with validated linearity (10–1000 ng/mL, R > 0.997), accuracy (relative error < ± 7.49%), and precision (RSD < 7.50%). The novelty of the assay is the harmonization of analytical performance with green analytical chemistry principles. The validated method provides a robust platform for studying monodisperse PEG derivatives while addressing growing demands for sustainable analytical technologies. Green analytical chemistry metric assessments confirmed the environmental sustainability of the method. Cellular pharmacokinetic analysis revealed time-/concentration-dependent uptake kinetics of HO-PEG 8 -OH polymers in MCF-7 cells, showing 3.2-fold accumulation between 0.5 and 48 h exposure. These findings offer important insights for PEG-based drug delivery system optimization and establish a new standard for environmentally conscious bioanalytical method development. Graphical
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DOI
PubMed
高影响因子
JOURNAL OF PHARMACY AND PHARMACOLOGY
·
2025
·
IF 3.2
Zhou Dan,He Kai,Cai Wei,Li Bin,Zhang Zaiqi
ObjectiveTo identify the anti-inflammatory ingredients of a typical Dong herbal medicine Jiao Mei Gu (JMG) (Cayratia albifolia C.L.Li) and reveal the underlying mechanisms.MethodsFor the first time, the chemical constituents in JMG ethyl acetate extract, which showed the highest anti-inflammatory activity, were analyzed by Ultra-performance liquid chromatography-quadrupole-electrostatic field Orbitrap mass spectrometry (UHPLC-Q-Exactive orbitrap MS). The anti-inflammatory activities and the underlying mechanisms of JMG extracts were evaluated in the lipopolysaccharide (LPS)-induced RAW 264.7 cell model and LPS (10 mg/kg) induced acute lung injury model in BALB/c mice.Key findingsOverall, 65 compounds including lignans, apigenin, quercetin, chrysin, phlorizin, and eriodictyol, etc., were identified in JMG ethyl acetate extract. At 200 mg/kg, JMG ethyl acetate extract reversed the structure change of lung alveoli and inflammatory cell infiltration in LPS-induced acute lung injury model. Compared with the LPS group, the serum levels of IL-1β, IL-6, and TNF-α in the 200 mg/kg JMG-treated group were decreased by 58.6%, 56.5%, and 87.6%, respectively. Western blot results revealed that JMG ethyl acetate extract inhibited LPS stimulated p65 and IκBα phosphorylation in mouse lung.ConclusionThe present study demonstrated that the ethyl acetate fraction of JMG could reverse LPS-induced acute lung hemorrhagic necrosis and inflammatory cell infiltration in mice by preventing the phosphorylation of NF-κB p65 and reducing its nuclear translocation.
研究领域:
生药学
·
民族药理学
·
分析化学
·
炎症研究
·
肺部医学
·
质谱分析
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2020
·
IF 5.339
Shi-En Chen,Jingwen Hu,Ping Yan,Jing Sun,Wenhui Jia,Shuyun Zhu,Xian-En Zhao,Huwei Liu
Urinary sarcosine was considered to be a potential biomarker for prostate cancer (Pca). In this work, an integrated strategy of multiplex tags chemical isotope labeling (MTCIL) combined with magnetic dispersive solid phase extraction (MDSPE), was proposed for specific extraction and high-throughput determination of sarcosine by ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). In the past three months, we have developed 8-plex MTCIL reagents with excellent qualitative and quantitative performance. In this work, the multiplexing capacity of MTCIL reagents (MTCIL360/361/362/363/364/365/366/375/376/378/379/381) was increased 1.5-fold from 8-plex to 12-plex. MTCIL359 was prepared and used to label sarcosine standard as internal standard (IS). The structural analogue derivative (MTCIL373-sarcosine) of all targeted MTCIL-sarcosine derivatives was synthesized and used as a novel dummy template to prepare dummy magnetic molecularly imprinted polymers (DMMIPs). The integration of MTCIL and DMMIPs procedures were extremely favorable to excellent chromatographic separation and efficient mass spectrometric detection. The labeling efficiency, chromatographic retention and mass spectrometry responses of MTCIL reagents were consistent for sarcosine. In a single UHPLC-MS/MS run (2.0 min), this method can simultaneously quantify sarcosine in 12-plex urine samples and achieve unbiased concentrations comparison between different urine samples. Analytical parameters including linearity (R 2 0.989–0.997), detection limits (0.02 nM), precision (2.6–11.5%), accuracy (96.1–107.4%), matrix effect, labeling and extraction efficiency were carefully validated. The proposed method was successfully applied for urinary sarcosine determination of healthy male individuals and Pca patients. It was found that the sarcosine concentrations in these two groups were statistically extremely significantly different ( P < 0.001). The developed method was a powerful analytical tool to substantially promote the analysis throughput and large-scale experiments about the potential biomarker research.
研究领域:
分析化学
·
医学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Qing Lu,Hao Guo,Yuanyuan Zhang,Xiaodong Tang,Weibin Lei,Ruijuan Qi,Junhao Chu,Dezeng Li,Qingbiao Zhao
Graphene oxide–Fe 3 O 4 (GO–Fe 3 O 4 ) nanocomposite was synthesized by a facile chemical co-precipitation method. The GO–Fe 3 O 4 was used as magnetic sorbent to extract the eight psychoactive drugs from urine samples. The analytes are morphine (MOR), 6-monoacetylmorphine (6-MAM), amphetamine (AMP), methamphetamine (MAMP), codeine, cocaine, dolantin and benzoylecgonine (BZE), which were determined by ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). This method has high selectivity for the target analytes. The limit of detection (LOD) and limit of quantification (LOQ) were 0.02–0.2 μg L −1 and 0.05–0.5 μg L −1 , respectively. The Mandel's fitting test revealed good linearity within all linear ranges. The linear ranges were calculated as 0.05–1000 μg L −1 for AMP, MAMP, cocaine and dolantin; 0.1–1000 μg L −1 for 6-MAM and codein; and 0.5–1000 μg L −1 for MOR and BZE. The recoveries ranged in 80.4–105.5%. The intra-day and inter-day RSDs are in the range of 2.7–13.1% and 3.9–13.7%, respectively. Magnetic solid phase extraction (MSPE) with GO–Fe 3 O 4 provides a convenient, rapid and green sample pretreatment method for extracting the target psychoactive drugs from urine. This methodology can be used for simultaneous or individual detection of eight major psychoactive drugs with high sensitivity. This method has high potential in clinical and forensic areas for psychoactive drugs analysis.
研究领域:
分析化学
·
法医学
·
临床检验
✓ 已验证
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）