SCIENCE OF THE TOTAL ENVIRONMENT
·
2022
·
IF 10.753
Zhi-Feng Chen,Ying-Tao Tang,Xiao-Liang Liao,Jie-Ru Jiang,Zenghua Qi,Zongwei Cai
Organophosphate flame retardants (OPFRs) have been widely used in consumer products to prevent fire spread. However, once released into the atmospheric environment, they may accumulate in humans and undergo metabolic transformation and excretion by urine. In order to clarify the human exposure to OPFRs, a quick, easy, cheap, effective, rugged, and safe method for the simultaneous determination of urinary OPFRs and their metabolites by ultra-performance liquid chromatography-tandem triple quadrupole mass spectrometry was developed. After the optimization by a single-factor or orthogonal experiment, the satisfactory recovery (87.8–119%), matrix effect (−8.88–9.29%), method quantitation limit (3.66–159 ng/L), and inter-day repeatability (1.24 − 10.6%) of most analytes were achieved in artificial urine samples. Based on a monitoring test by the developed method, we propose that urinary bis(1-chloro-2-propyl) phosphate and di- p -cresyl phosphate could be used to trace human exposure to tris(1-chloro-2-propyl) phosphate and tricresyl phosphate, respectively. Most importantly, this is the first study to reveal that 4-hydroxyphenyl diphenyl phosphate (4-OH-TPHP) was dominantly presented in its conjugated form rather than its free form in urine ( p = 0.037). Overall, the obtained results contribute a relatively rapid method to help conduct large-scale urine monitoring for revealing the human exposure and risk of OPFRs.
研究领域:
分析化学
·
环境科学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Chemistry
·
2025
·
IF 4.2
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.
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
Heliyon
·
2023
·
IF 4
Huaxi Liu,Weijie Chen,Chunyang Tian,Yijian Deng,Liangwo Xu,Wenkun Ouyang,Renjie Qiu,Yanting You,Pingping Jiang,Lin Zhou,Jingru Cheng,Hiu Yee Kwan,Xiaoshan Zhao,Xiaomin Sun
Background IgA nephropathy (IgAN) is a major and growing public health problem. Renal fibrosis plays a vital role in the progression of IgAN. This study is to investigate the mechanisms of action underlying the therapeutic effects of Shenbing Decoction II (SBDII) in IgAN renal fibrosis treatment based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), network pharmacology and experimental verification. Method We first used UPLC-MS/MS to explore the main compounds of SBDII, and then used network pharmacology to predict the targets and key pathways of SBDII in the treatment of IgAN renal fibrosis. Next, bovine serum albumin (BSA), lipopolysaccharide (LPS), and carbon tetrachloride (CCL4) were used to induce IgAN in rats, and then biochemical indicators, renal tissue pathology, and renal fibrosis-related indicators were examined. At the same time, part of the results predicted by network pharmacology were also verified. Result A total of 105 compounds were identified in SBDII by UPLC-MS/MS. Network pharmacology results showed that the active compounds such as acacetin, eupatilin, and galangin may mediate the therapeutic effects of SBDII in treating IgAN by targeting tumor protein p53 (TP53) and regulating phosphatidylinositol 3-kinase (PI3K)-Akt kinase (Akt) signaling pathway. Animal experiments showed that SBDII not only significantly improved renal function and fibrosis in IgAN rats, but also significantly downregulated the expressions of p53, p-PI3K and p -Akt. Conclusion This UPLC-MS/MS, network pharmacological and experimental study highlights that the TP53 as a target, and PI3K-Akt signaling pathway are the potential mechanism by which SBDII is involved in IgAN renal fibrosis treatment. Acacetin, eupatilin, and galangin are probable active compounds in SBDII, these results might provide valuable guidance for further studies of IgAN renal fibrosis treatment.
研究领域:
药理学
·
肾病学
·
分子生物学
·
中医药
✓ 已验证
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2025
·Vol. 40
·期 1
·e70254
·
IF 1.7
Jie Shen,Lin Zhang,Jianbang Wu,Yan Zhou,Minhui Wang,Changmao Wang,LingLing Zhu,Yaqin Wang,Ping Wu,Xiaocui Xia,Wanyu Wang,Yamin Liu,Yuanwei Jia
A simple, sensitive and efficient ultra performance liquid chromatography–mass spectrometry (UPLC–MS/MS) method for simultaneous quantitative determination of olmesartan and hydrochlorothiazide in human plasma has been developed and validated. Using olmesartan-d 4 and hydrochlorothiazide- 13 C-d 2 as stable isotope-labeled internal standard (SIL-IS). Plasma samples were processed by protein precipitation. Separated on a ZORBAX Eclipse XDB-Phenyl column (150 mm × 4.6 mm, 5 μm) using a gradient elution with mobile phases methanol and 5 mM ammonium acetate. Detected by electrospray ionization (ESI) in negative ion mode of multiple reaction monitoring (MRM), mass transition ion pairs were m/z 445.1 → 149.0 for olmesartan, m/z 295.9 → 204.9 for hydrochlorothiazide, m/z 449.1 → 149.1 for olmesartan-d 4 , and m/z 301.0 → 272.0 for hydrochlorothiazide- 13 C-d 2 . Linear ranges were 10–2000 ng/mL for olmesartan and 1.5–300 ng/mL for hydrochlorothiazide. Mean recoveries of olmesartan, hydrochlorothiazide, olmesartan-d 4 , and hydrochlorothiazide- 13 C-d 2 were 91.31%, 99.34%, 92.62%, and 98.61%, respectively. Our method was well validated in selectivity, carryover, lower limit of quantification (LLOQ), calibration curve, accuracy, precision, dilution effect, matrix effect (normal, hyperlipidemic, and hemolyzed matrices), stability, recovery, and IRS. It was successfully applied in a bioequivalence study of olmesartan medoxomil and hydrochlorothiazide tablets (20/12.5 mg) in healthy Chinese volunteers.
研究领域:
药物分析
·
临床药理学
·
生物分析化学
·
色谱-质谱分析
✓ 已验证
产品关联
DOI
PubMed
高影响因子
BIOMEDICAL CHROMATOGRAPHY
·
2026
·Vol. 40
·期 8
·e70547
·
IF 1.7
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.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Heliyon
·
2024
·
IF 3.4
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
MICROCHEMICAL JOURNAL
·
2025
·
IF 5.1
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
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2015
·
IF 2.729
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
DYES AND PIGMENTS
·
2026
·
IF 3.9
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
BIOMEDICAL CHROMATOGRAPHY
·
2020
·Vol. 35
·期 3
·e4991
·
IF 1.728
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.
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
Food Additives and Contaminants Part A-Chemistry Analysis Control Exposure & Risk Assessment
·
2018
·
IF 2.129
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.
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
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2022
·
IF 3.318
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.
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
危险品化学品经营许可证（带存储）