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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2015 · IF 2.729

An UPLC-MS/MS method for determination of solasonine in rat plasma and its application of a pharmacokinetic and bioavailability study

Yuanyuan Chen,Shuangshuang Zhang,Dahui Chen,Mi Zhou,Jing Zheng,Zheng Xiang

Solasonine, a known glycoalkaloid, is a potential anti-cancer agent. In this work, a simple, sensitive and fast ultra performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantitative determination of solasonine in rat plasma. Plasma samples were processed with a protein precipitation. The separation was achieved by an ACQUITY HSS T3 (100   ×   2.1   mm, 1.8   μm) column with a gradient mobile phase consisting of 0.1% formic acid and acetonitrile. Detection was carried out using positive-ion electrospray tandem mass spectrometry via multiple reaction monitoring (MRM). The validated method had an excellent linearity in the range of 0.1–500   ng/mL ( R 2   >   0.994) with a low limit of detection (0.1   ng/mL) and lower limit of quantification (0.5   ng/mL). The extraction recovery was in the range of 92.4–94.9% for solasonine and 91.9% for dendrobine (internal standard, IS). The intra- and inter-day precision was below 9.8% and accuracy was from 86.0% to 94.3%. No notable matrix effect and astaticism was observed for solasonine. The method has been successfully applied to a pharmacokinetic and bioavailability study of solasonine in rats for the first time, which provides the basis for the further development and application of solasonine.

研究领域: 药物分析 · 药代动力学 · 分析化学 · 天然产物 · 肿瘤学
✓ 已验证 DOI 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2026 ·Vol. 40 ·期 8 ·e70547 · IF 1.7

Development and Validation of a UPLC–MS/MS for Determination of Loureirin D in Rat Plasma and Its Application to Pharmacokinetics

Yi Zhou,Yuxin Wu,Chenyao Xu,Chenbin Zhang,Congcong Wen,Xianqin Wang,Jianbo Li

Loureirin D is a bioactive dihydrochalcone isolated from Dracaena resin with very high therapeutic value. A sensitive and high-throughput ultra-performance liquid chromatography–mass spectrometry (UPLC–MS/MS) method was developed for the quantitative analysis of loureirin D in rat plasma with only 50 μL of sample per assay. Sample extraction was protein precipitation using acetonitrile, and isoscoparin was used as internal standard (IS). Separation was achieved on the BEH C18 column with a gradient mobile phase of 0.1% (v/v) aqueous formic acid and acetonitrile. Detection was achieved with negative-ion electrospray ionization (ESI) detector in the multiple reaction monitoring (MRM) mode. The method was validated and proved to be linear in the concentration range of 2–2400 ng/mL ( r ≥ 0.995), intraday and interday precision (RSD) was < 15%, and accuracy was 93.3%–110.1%. The extraction recovery was 88.7%–94.4%, and the matrix effects were 87.3%–92.9%. UPLC-MS/MS was used in pharmacokinetics in the rats after administration of loureirin D. The AUC (0– t ) after intravenous administration (1 mg/kg) was 2074.7 ± 180.3 ng · h/mL, and AUC (0– t ) after oral administration (5 mg/kg) was 563.4 ± 61.4 ng · h/mL; the absolute oral bioavailability was 5.4%. Pharmacokinetics showed rapid absorption, large V z / F (52.7 ± 10.7 L/kg), high CL z / F (8.8 ± 0.9 L/h/kg), and extensive first-pass metabolism.

CAS / MDL: 64-18-6
✓ 已验证 产品关联 DOI PubMed 高影响因子
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DYES AND PIGMENTS · 2026 · IF 3.9

Elucidating the Hue Shift and Metal Coordination Mechanism of Traditional Sappanwood Mordant Dyeing on Silk via UPLC–MS/MS and DFT

Panpan Zhu,Yahui Tao,Huihui Wu,Feng Zhao

Understanding the chromogenic and dye-metal chelation mechanisms in sappanwood ( Caesalpinia sappan L. ) dyeing is fundamental to the precise conservation of silk heritage and the optimization of modern botanical dyeing. Herein, three distinct hues of sappanwood-dyed silk were reconstructed via traditional techniques, and brazilein coordination behaviors with two mordants were systematically investigated. It was found that the introduction of alum and ferrous sulfate mordants induced a significant hue transition of the dyed silk from the native orange to vivid red and deep purple-black, respectively. Density Functional Theory (DFT) calculations further revealed that brazilein exists as the ring A-deprotonated monoanion in neutral solution. Based on this, thermodynamic analysis indicated that the Al 3+ -mordanted system exhibits the coexistence of trans- like and cis- like configurations, while the Fe 3+ -mordanted system is dominated by a single trans- like configuration. Hole-electron analysis demonstrated that the vivid red color arises from the electrostatic field effect of closed-shell Al 3+ , while the deep purple-black originates from the mixed charge transfer of open-shell Fe 3+ causing spectral broadening. Furthermore, the proposed coordination models and excited-state analysis successfully explained the trends observed in the experimental UV-vis absorption spectra upon mordanting. In summary, this study elucidates the metal chelation and chromogenic mechanisms of sappanwood dyeing at the molecular level, providing a theoretical basis for conserving textile heritage and advancing modern botanical dyeing.

✓ 已验证 产品关联 DOI 高影响因子
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Heliyon · 2024 · IF 3.4

Quantification of meropenem in serum and cerebrospinal fluid in children with bacterial meningitis with augmented renal clearance by UPLC–MS/MS

Ying Jin,Hongtu Ma,Lisha Fu,Xiaohui Qi,Mengyu Zhang,Xiangjie Di,Li Zheng,Cuiyao He,Zhenlei Wang

Meropenem is an ultrabroad-spectrum antimicrobial agent that is often recommended for the treatment of bacterial meningitis (BM) in children. However, a subtherapeutic phenomenon occurred in BM children complicated with augmented renal clearance (ARC) at the recommended dose of meropenem. To support its pharmacokinetics, a sensitive, fast and robust ultra-liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) method was developed to measure meropenem concentrations in serum and cerebrospinal fluid (CSF). The method involved protein precipitation, and samples were diluted with a large proportion of water to eliminate solvent effects. The separation of samples was performed on a Waters Acquity™ BEH C 18 column (2.1 × 50 mm i.d., 1.7 μm) with a gradient profile. The mobile phases were formic acid–water (1:1000, v/v) and acetonitrile. The linear range was good, with a concentration range of 0.100–100 μg/mL for serum and 0.0400–20.0 μg/mL for CSF. The intra-day and inter-day precisions were less than 8.0%, and the intra-day and inter-day accuracies varied −6.6% from 6.5% for the both serum and CSF. The selectivity, carry-over, dilution integrity, matrix effect, recovery and stability were validated according to international guidelines. The developed UPLC–MS/MS method successfully determined the meropenem concentrations in the serum and CSF of children with BM complicated with ARC. The results indicated that under the recommended dosing regimen (40 mg/kg every 8 h), the time to reach the effective treatment target of 50%T > MIC was only approximately 3 h and lower CSF concentrations of meropenem were observed in children with BM with ARC.

研究领域: 药代动力学 · 临床药学 · 分析化学 · 儿科
✓ 已验证 DOI PubMed 高影响因子
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MICROCHEMICAL JOURNAL · 2025 · IF 5.1

Detection of antidepressants in wastewater from four provinces of China by UPLC-MS/MS to assess the regional prevalence of depression

Moying Yang,Yan Yao,Haotian Shen,Fei Teng,Yunuo Liu,Yuyang Ma,Bin Di,Mengxiang Su

Depression has gradually become a serious public health problem. Traditionally, data on depression are mainly derived from questionnaires or antidepressant prescriptions, and these methods may suffer from update delays and survey bias, resulting in a low actual prevalence of depression. To monitor the prevalence of depression in near real-time, this study developed an analytical method of UPLC-MS/MS by wastewater-based epidemiology to detect 10 typical antidepressants and metabolites in four provinces of China. The method has high sensitivity in that the lower limit of quantification was 2 ng/L. And the method provides recoveries and matrix effects ranging from 85.12 % to 102.98 % and 84.95 % to 112.75 %, respectively. The results showed that among the four provinces, the highest average detected concentration of antidepressants was in Jiangsu (91.82 ± 150.46 ng/L), followed by Guangxi (76.06 ± 130.44 ng/L), Anhui (61.53 ± 94.09 ng/L), and Hainan (27.87 ± 28.33 ng/L). Most wastewater treatment facilities had antidepressants such as venlafaxine, fluvoxamine, and agomelatine. The average back-calculated consumption of venlafaxine and fluvoxamine was 815.88 ± 2015.96 mg/day/1000 inh and 497.02 ± 405.21 mg/day/1000 inh, respectively. Based on this study, the estimated prevalence in the population over 15 in Jiangsu, Anhui, and Hainan was finally determined to be 4.90 %, 5.36 %, and 2.93 %, indicating regional diversity. This study offered a workable way to track the prevalence of depression using wastewater-based epidemiology, which aided public health agencies in comprehending the state of depression prevalence.

研究领域: 环境科学 · 分析化学 · 流行病学 · 公共卫生 · 药物监测
✓ 已验证 产品关联 DOI 高影响因子
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BIOMEDICAL CHROMATOGRAPHY · 2020 ·Vol. 35 ·期 3 ·e4991 · IF 1.728

A UPLC–MS/MS method for determination of endogenous l-carnitine and acetyl-l-carnitine in serum of patients with depression

Li-Juan Nie,Jun Liang,Feng Shan,Ya-Yun Xu,Chun-Yu Yan,Xuan Zhou,Zhuo-Yu Cheng,Qing-Rong Xia

A simple, rapid, and selective ultra-performance liquid chromatography–tandem mass spectrometry method for determination of l -carnitine (LC) and acetyl- l- carnitine (ALC) in human serum was developed. Acetyl- l- carnitine-d 3 (ALC-d 3 ) was selected as internal standard (IS). After protein precipitation with acetonitrile–water (1 mL, 2:1, v/v), the analytes and IS were separated on a 2.5-μm XSelect HSS T3 C 18 column by gradient elution with methanol–water (containing 0.01% ammonia water) as the mobile phase at a flow rate of 0.2 mL/min. Analytes were detected with multiple reaction monitoring using a positive scan mode with electrospray ionization. Good linearity ( R 2 > 0.999) was observed in the concentration range for LC and ALC. The inter- and intra-day values of relative error were −10.4% to 10.0% with CVs less than 9.84%. The average recoveries of the two analytes were 91.29%–98.23%. Blood samples containing LC and ALC were stable under various storage conditions. Normal, haemolytic, and hyperlipidaemic serum had no significant effect on the quantification of LC and ALC. This method was successfully applied to study the concentrations of endogenous LC and ALC in the serum of patients with first-episode depression.

CAS / MDL: 1336-21-6
研究领域: 分析化学 · 医学 · 精神健康研究
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Frontiers in Chemistry · 2025 · IF 4.2

Establishment and evaluation of a UPLC-MS/MS method for simultaneous determination of bongkrekic acid and dehydroacetic acid in rice noodles

Lingguo Zhao,Ronggui Lv,Jiang Song,Xi Chen,Lei Lei,Weixian Zeng,Miaowen She,Dabing Li,Xiaxia Yu,Zhanguo Liu,Xiao Wang,Yong Liu

A UPLC-MS/MS method with one-step extraction and simultaneous determination of bongkrekic acid (BA) and dehydroacetic acid (DHA) in rice noodles has been established in this study for the first time. The extraction solvent consisted of a mixture of methanol, ammonia, and water. Electrospray ionization negative ion mode (ESI-) was used for multiple reaction detection and external standard method was used for quantitative determination. The method demonstrated a good linearity range of 0–50 ng/mL with a correlation coefficient (r) of 0.9998 for BA, and showed a linearity range of 0∼500 ng/mL with r of 0.9993 for DHA. The limits of detection (LOD) were determined to be 0.1 μg/kg for BA and 0.6 μg/kg for DHA. Additionally, the method exhibited good recovery of 90.1%∼105.4% for BA and 80.4%∼102% for DHA. Meanwhile, the method also exhibited good precision with RSD of 0.4%∼7.5% for BA, and with RSD of 4.5%∼11.4% for DHA. Furthermore, the established method was sucessfully applied to the analysis of rice noodles from two production enterprises. BA was detected in one rice noodle sample and DHA was detected in 7 rice noodle samples in the enterprises A which was the manufacturer of food consumed by the poisoned patient. To investigate the cause of death of the poisoned patient, the toxigenic bacterium Burkholderia gladiolus was isolated and cultured to produce BA. The results showed that the established method could also be used to qualitatively screen BA and its isomer isobongkrekic acid (IBA) in GVC enrichment broth, potato glucose agar and rice sample, which facilitates a rapid and accurate judgement of whether the isolated bacterium strain produces BA. With high sensitivity and accuracy, and simple sample pretreatment, the proposed method shows potential for safety assessment of the entire production process of rice-derived products, addressing a significant public health concern.

CAS / MDL: 64-19-7
研究领域: 食品安全 · 分析化学 · 微生物学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment · 2018 · IF 2.129

Fast simultaneous determination of capsaicin, dihydrocapsaicin and nonivamide for detecting adulteration in edible and crude vegetable oils by UPLC-MS/MS

Chuan Zhou,Dianping Ma,Wenming Cao,Haiming Shi,Yuanrong Jiang

Capsaicinoids are pungent components in hot peppers, which have been detected in waste cooking oil. However, trace analysis of capsaicinoids in edible and crude vegetable oils is a challenging task due to the complex matrix. In this study, a simple liquid-liquid extraction and solid phase extraction (SPE) coupled with RP-UPLC-ESI-MS/MS method was developed for the quantification of capsaicinoids in edible and crude vegetable oils to screen the adulteration with waste cooking oil. This method was used to simultaneously determine 3 capsaicinoids (capsaicin, dihydrocapsaicin, and nordihydrocapsaicin) with capsaicin-d3, and dihydrocapsaicin-d3 as internal standards. This method allows the complete analysis of a sample in only an hour, even including sample preparation and chromatographic separation. The linear range of 3 capsaicinoids ranged between 0.5 and 40 µg/kg. The limit of detection (LOD) and limit of quantification (LOQ) for capsaicinoids were calculated as 0.15 and 0.5 µg/kg, respectively. Quantitative recoveries ranging from 92.9% to 105% were obtained by the analysis of spiked oil. The relative standard deviations were less than 5% (n = 6). The established method can potentially overcome the interference of triacylglycerols and fatty acids in edible and crude vegetable oils, and have been successfully applied to analyse real oil samples. This method provided a rapid and reliable method for the detection of adulteration of vegetable oils with waste cooking oils.

CAS / MDL: 2444-46-4
研究领域: 食品科学 · 分析化学
✓ 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 · 2022 · IF 3.318

A sensitive and rapid bioanalytical method for the quantitative determination of luliconazole in rabbit eye tissues using UPLC-MS/MS assay

Jingjing Yang,Zhen Liang,Ping Lu,Fei Song,Zhen Zhang,Huiyun Xia,Jijun He,Tianyang Zhou,Junjie Zhang

Luliconazole (LCZ) is a novel antifungal imidazole with broad-spectrum and high susceptibility of Aspergillus and Fusarium are the dominant species of fungal keratitis, may potentially be a new medical treatment option for ocular fungal infection. To evaluate LCZ distribution in ocular tissues after topical application for the development of ophthalmic delivery system, it is important to have a bioanalytical method for measuring the drug concentrations in different ocular tissues and aqueous humor (AH). A selective and sensitive ultrahigh performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of LCZ in rabbit ocular tissues, including conjunctiva, cornea, AH, iris, lens, vitreous humor (VH), retinal choroid and sclera, using lanoconazole as internal standard (IS). Chromatographic separation was achieved on a Xterra MS, C18 column (2.1 × × 50 mm, 3.5 μm) using mobile phase with formic acid solution (0.2%, v/v): acetonitrile (50:50, v/v) at a flow rate of 0.2 ml/min, and the run time was 2.5 min. Detection was performed using the transitions 354.1 → → 150.3  m / z for LCZ and 320.1 → → 150.3  m / z for IS by positive ion electrospray ionization in multiple reaction monitoring (MRM) mode. Method validation was conducted in accordance with U.S. Food and Drug Administration’s regulatory guidelines for bioanalytical method validation. The calibration curves were linear over the concentration range from 2.80 ng/ml to 2038 ng/ml for conjunctiva, cornea and sclera, 2.09 ng/ml to 1019 ng/ml for AH, 2.09 ng/ml to 509.5 ng/ml for iris, 2.09 ng/ml to 203.8 ng/ml for retinal choroid and VH, 2.04 ng/ml to 101.9 ng/ml for lens, with all the squared correlation coefficients (r 2 ) more than 0.99. The accuracy of the method was within the acceptable limit of 89.34%∼112.78% at the lower limit of quantification and other concentrations, Inter-day and intra-day precision values, expressed in terms of RSD (%), in all tissues were within 15% at all concentrations. The mean recoveries of LCZ in rabbit ocular tissues was 84.85%∼100.52%. No interference was found due to matrix components. Luliconazole was stable during the stability studies, including autosampler stability, benchtop stability, freeze/thaw stability and long-term stability. The method was successfully applied to the ocular pharmacokinetic and tissues distribution studies of LCZ in rabbit after topical administration of LCZ ophthalmic drug delivery system.

CAS / MDL: 64-18-6
研究领域: 药理学 · 分析化学 · 眼科
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ACS Omega · 2023 · IF 4.1

Determination of the Dissipation Dynamics and Terminal Residue of Bupirimate and Its Metabolites in Cucumber by QuEChERS-Based UPLC-MS/MS

Yue Chen,Deliang Gao,Yueming Wu,Ling Wang,Weidi Fan,Yun Gao,Wenli Wang,Li Su,Beixing Li,Wei Mu,Weili Yu

Bupirimate is widely used as a highly active systemic fungicide. However, the frequent and heavy use of bupirimate has led to pesticide residues in crops that threaten human health and food safety. At present, there is limited research on the detection of ethirimol, which is the metabolite of bupirimate. This study established an ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method to simultaneously detect bupirimate and ethirimol residues based on QuEChERS pretreatment. The average recoveries of bupirimate and ethirimol in cucumber were between 95.2 and 98.7%, respectively, with relative standard deviations (RSDs) of 0.92–5.54% at fortified levels of 0.01, 0.1, and 5 mg L–1. The established method was used to determine the residues in field trials in 12 regions of China, and the final residues of bupirimate were all less than the maximum residue limit (MRL). Since the risk quotient (RQ) of bupirimate and ethirimol in cucumber was less than 1.3%, the dietary risk assessment indicated that bupirimate and ethirimol had a low long-term dietary risk to the general population in China. This study provides effective guidance on the proper use of bupirimate in cucumber fields and a reference for establishing the MRL of bupirimate in China.

CAS / MDL: 64-18-6
研究领域: 植物保护 · 食品安全 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Foods · 2023 ·Vol. 12 ·期 17 ·3236 · IF 5.2

Extract of Pfaffia glomerata Ameliorates Paroxetine-Induced Sexual Dysfunction in Male Mice and the Characterization of Its Phytoconstituents by UPLC-MS

Qianqian Huang,Haiying Wu,Xiaoming Qin

Pfaffia glomerataextract (PGE) has a variety of biological activities. However, its ameliorative effect on and exact working mechanism in male sexual dysfunction are still poorly understood. This study aims to evaluate the ameliorative effect of PGE on paroxetine (PRX)-induced sexual dysfunction in male mice and uses molecular docking technology to investigate its underlying mechanism. In this work, PRX-induced sexual dysfunction was caused and PGE was gavaged in mice for 28 days. The results show that PGE significantly improved the sexual performance of mice and reduced the damage to testicular tissues. Further studies showed that PGE restored serum sex hormones to normal levels and increased nitric oxide (NO) and cyclic guanosine monophosphate (cGMP) levels as well as nitric oxide synthase (NOS) activity in penile tissues, while also decreasing phosphodiesterase-5 (PDE-5) activity, thereby maintaining normal penile erection in mice. In addition, PGE improved the activities of enzymes (LDH, ACP, and ALP) related to energy metabolism in the testis and significantly increased sperm count and viability in mice. Furthermore, the molecular docking results show that all eight compounds in PGE could form a stable complex with PDE-5 and inhibit the activity of PDE-5. In conclusion, PGE had an ameliorative effect on PRX-induced sexual dysfunction, suggesting that PGE has a potential protective effect on male sexual health.Keywords:Pfaffia glomerata;extract;sexual function;molecular docking;paroxetine

CAS / MDL: 5289-74-7
研究领域: 药理学 · 性健康 · 分子生物学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD CHEMISTRY · 2021 · IF 7.514

Non-volatile and volatile metabolic profiling of tomato juice processed by high-hydrostatic-pressure and high-temperature short-time

Xuehua Wang,Fang Chen,Lingjun Ma,Xiaojun Liao,Xiaosong Hu

High hydrostatic pressure (HHP) processing has become a commercial success in fruit and vegetable processing. Herein, the effects of HHP and high-temperature short-time (HTST) processing on metabolic profiling in tomato juice was evaluated by UPLC–MS/MS, HPLC, and GC–MS; a total of 425 metabolites, 14 carotenoids, and 56 volatile compounds were identified in tomato juice. HHP processing affects the composition of the juice less than HTST processing, considering 4 and 33 differential metabolites discriminated after HHP and HTST processing, respectively. The total lycopene and carotenoid contents in tomato juice increased after HHP processing, while the β-carotene and lycopene contents decreased after HTST processing. Further, more volatile compounds and higher contents of aldehydes that contribute to green aroma and lower contents of alcohols were observed after HHP and HTST processing, respectively. These findings provide a comprehensive understanding of the advantages of HHP processing on metabolite profiles in tomato juice.

CAS / MDL: 7235-40-7
研究领域: 食品科学 · 分析化学 · 营养学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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