Current Pharmaceutical Analysis
·
2023
·Vol. 19
·期 6
·511-520
·
IF 0.6
Zhang Mengmeng,Zou Qiaogen
Background: Atopic dermatitis (AD) is an allergic skin disease that can be inherited. Crisaborole is a specific drug developed to deal with this disease. The compounds of 4-(4- Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4-bromo-3-formylphenoxy)-3- formylphenoxy) benzonitrile
are the representative impurities in the synthesis of Crisaborole active pharmaceutical in gradient (API). Owing to the genotoxic impurities that could lead to cancer and gene mutations, it is necessary to develop a simple, efficient, sensitive, and accurate method to detect these impurities.
In this study, the 4-(4-Bromo-3-formyl-phenoxy)-benzonitrile and 4-(4-(4- bromo-3-formylphenoxy)-3-formylphenoxy)benzo- nitrile present in Crisaborole API were detected using UPLC-MS/MS. Methods: The separation was made on a ZORBAX Eclipse XDB-Pheny column (4.6 mm ×75mm, 3.5
μm) with the mobile phase of acetonitrile solution containing 0.1% trifluoroacetic acid (A) and water containing 0.1% formic acid (B) in gradient elution mode. Quantification was performed using positive ion electrospray ionization (ESI), and the contents of two compounds were determined
using the multiple reaction monitoring (MRM) modes. Results: The quantitative analytical method was fully validated with respect to linearity (r > 0.9998), sensitivity, precision, accuracy (the average recovery of two impurities was 84.1% to 90.7%), and robustness. Conclusion:
Three batches of samples were detected by UPLC-MS/MS, indicating that the proposed approach was applicable for the quality evaluation of Crisaborole.
研究领域:
药物分析
·
皮肤病学
·
毒理学
✓ 已验证
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Yan Qiao,Menglin Wang,Erling Guo,Ke Wang,Ling Ma,Kaoqi Lian
This study aimed to design and synthesize a novel adsorbent Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material for the first time and used as an adsorbent of MSPE. It had significant potential for the pretreatment of trace analytes. The MSPE was coupled with ultra performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) for the rapid extraction and detection of 12 sulfonamides (SAs) from water and milk samples for the first time. Several experimental parameters were optimized, including adsorbent dosage and the effects of pH, ionic strength, adsorption time, and desorption conditions. Under the optimized pretreatment and instrumental conditions, good linearity of 0.1–100 μg·L −1 with a correlation coefficient 0.9994–0.9999, low limits of detection (0.004–0.044 μg·L −1 ) and limits of quantitation (0.013–0.136 μg·L −1 ) were obtained. Moreover, the recoveries of sulfonamides in water and milk samples were in the range of 60.88 %-102.94 %, and the relative standard deviations not exceeding 9.62 %. Finally, the magnetic Fe 3 O 4 @SiO 2 @MPA-TAPA-COF material possessed the magnetic separation and high adsorption affinity for extracting SAs from real samples. This study holds great significance in enhancing the monitoring of SAs drug residues in water and milk.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2017
·
IF 3.255
Xiaoxue Liu,Chenrong Huang,Ling Xue,Qingqing Xu,Wen Xia,Xing Li,Liyan Miao
A rapid and highly sensitive liquid chromatography-tandem mass spectrometry (LC–MS/MS) method has been developed and validated for the determination of a novel anti-HBV compound Y101 and its metabolites M8 and M9 in human plasma. The plasma samples were deproteinated with acetonitrile after addition of Peramivir (internal standard, IS) and separated on a 40 °C ACQUITY UPLC BEH C 18 column (2.1 mm × 50 mm, 1.7 μm). The mobile phase consisted of water (containing 5 mM ammonium acetate and 0.1% formic acid) and acetonitrile (74:26, v/v) at a flow rate of 0.3 mL/min. The detection was performed on a Triple Quad 5500 tandem mass spectrometer coupled with electrospray ionization (ESI) source in positive mode. Quantification was conducted by multiple reaction monitoring (MRM) of the transitions of m / z 490.1 → 339.0 for Y101, m / z 357.2 → 105.2 for metabolite M8, m / z 373.1 → 105.1 for metabolite M9 and m / z 329.1 → 270.2 for IS, respectively. The method was validated over the calibration curve range of 1.000–1000 ng/mL for Y101, 2.000–2000 ng/mL for metabolite M8 and 0.3000–300.0 ng/mL for metabolite M9, using linear regression and 1/x 2 weighting. No matrix effect and carryover effect was observed. The intra- and inter-batch precision and accuracy of Y101, metabolite M8 and M9 were all within the acceptable criteria. This method allows a rapid and simple determination of Y101 and its metabolites M8 and M9 in human plasma. It was successfully applied in a pharmacokinetic study in human for the first time.
研究领域:
药理学
·
分析化学
·
临床药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Weihao Ma,Hao Zhang,Jiayuan Nie,Chunyu Qiang,Zhiwei Li,Ling Ma,Ke Wang
In this study, a novel magnetic covalent organic framework (Fe 3 O 4 @SiO 2 -HBTA-TTA-COF) was synthesized, which was fully characterized by scanning electron microscopy, transmission electron microscopy, etc. Furthermore, a new method was developed for the determination of 25 quinolones (QNs) in water and milk using the Fe 3 O 4 @SiO 2 -HBTA-TTA-COF as magnetic solid-phase extraction adsorbent coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Meanwhile, various experimental parameters were optimized including sample solution pH, adsorbent dosage and extraction time, etc. Under the optimal conditions, good linearity in the range of 0.1–200 μg·L −1 (R 2 ≥ 0.999) were obtained, the recoveries of 25 QNs were 70.04 %–104.4 % with the relative standard deviations lower than 9.87 % (n = 5), the limits of detection were 0.003–0.010 μg·L −1 for water and 0.018–0.722 μg·kg −1 for milk. This established method was high-sensitive and high-throughput, which can be used as a good alternative method for the selective determination of 25 QNs in water and milk.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2015
·
IF 2.979
Min Liao,Cong Dai,Mengping Liu,Jiefeng Chen,Zuanguang Chen,Zhiyong Xie,Meicun Yao
A novel, sensitive and rapid ultra-performance liquid chromatography–tandem mass spectrometric (UPLC–MS/MS) method for simultaneous quantification of four furostanol glycosides in rat plasma was established and validated. Ginsenoside Rb1 was used as an internal standard. Plasma samples were pretreated by liquid–liquid extraction with n -butanol and chromatographed on a C18 column (2.1 × 50 mm i.d., 2.6 μm) using a gradient elution program consisting of acetonitrile and water (containing 0.03% formic acid and 0.1 mM lithium acetate) at a flow rate of 0.4 mL/min. Lithium adduct ions were employed to enhance the response of the analytes in electrospray positive ionization mode and multiple reaction monitoring transitions were performed for detection. All calibration curves exhibited good linearity ( r > 0.999) over the range of 10–20,000 ng/mL for protodioscin and 2–4000 ng/mL for protogracillin, pseudoprotodioscin and pseudoprotogracillin. The recoveries of the whole analytes were more than 80.3% and exhibited no severe matrix effect. Meanwhile, the intra- and inter-day precisions were all less than 10.7% and accuracies were within the range of −8.1–12.9%. The four saponins showed rapid excretion and relative high plasma concentrations when the validated method was applied to the PK study of Dioscorea nipponica extracts by intragastric administration at low, medium and high dose to rats. Moreover, the T 1/2 and AUC 0– t of each compound turned out to behave in a dose-dependent pattern by comparing them at different dose levels.
研究领域:
分析化学
·
药理学
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
·
2016
·
IF 4.035
Xinpeng Dai,Xiuna Jia,Pan Zhao,Ting Wang,Jian Wang,Peiting Huang,Lu He,Xiaohong Hou
As a novel kind of materials, metal-organic frameworks (MOFs) have great potential for the preconcentration of trace analytes. In our work, MIL-101(Cr) was prepared and applied as a solid phase extraction (SPE) sorbent for the pretreatment of sulfadiazine (SDA), sulfamethazine (SMZ), sulfachloropyridazine (SCP) and sulfamethoxazole (SMX) in different environmental water samples coupling with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) detection. Experimental parameters, such as SPE materials, pH of water sample, volume of sample, flow rate , and type and volume of elution solvent, were properly optimized. Under the optimum conditions, good sensitivity levels were achieved with the detection limits of 0.03–0.08 μg/L and the quantitation limits of 0.11–0.27 μg/L. The linear ranges were from 0.2–40 or 0.5–100 μg/L ( r 2 >0.996) for the analytes, and the relative recoveries were in the range from 83.5% to 107.3% with the relative standard deviations (RSD) between 0.2% and 8.0% ( n =6). In addition, computational simulation was primarily used to predict the adsorption of MIL-101(Cr) toward sulphonamides (SAs), and also demonstrated the molecular interactions and free binding energies with the molecular modeling method. The results revealed that the combination of experimental and computational study not only accurately recognized the adsorption of MIL-101(Cr) on SAs, but also provided a new strategy on the trace contaminant analysis.
研究领域:
环境科学
·
分析化学
✓ 已验证
DOI
高影响因子
Analytical Methods
·
2025
·
IF 2.6
Jieting Zhang,Shuo Diao,Zhen Huang,Mengyuan Wu,Xintong Wang,Yiran Zhao,Mingming Yu,Xianzhen Wang,Jingchun Yao,Guimin Zhang,Sherwin K. B. Sy,Zhihua Lv,Hai Yang
Guided by the principles of Analytical Quality by Design (AQbD), a highly selective and sensitive LC-MS/MS method was established for the simultaneous quantification of 15 compounds in Shouhui Tongbian capsules, enabling their effective quality control. The separation was carried out on a BEH C18 column (1.7 μm, 2.1 × 100 mm) with a mobile phase comprising 0.1% formic acid in 3 mM ammonium acetate aqueous solution and methanol (60 : 40, v/v) at a flow rate of 0.30 mL min−1. The method exhibited good linearity within a certain concentration range (R2 > 0.9906) depending on the compound; the precision ranged from 0.6% to 14.7% and accuracy was within 11.2%. Among the 15 detected compounds, aloin had the highest content in the Shouhui Tongbian capsules, reaching 227.3780 mg g−1, followed by betaine and L-hydroxyproline, with concentrations of 1.3204 mg g−1 and 1.2929 mg g−1, respectively. This method simultaneously detected the content of 15 compounds in five batches of Shouhui Tongbian capsules.
研究领域:
分析化学
·
药物分析
·
质量控制
·
色谱-质谱分析
·
中医药学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2021
·
IF 3.935
Menghua Zhang,Xiaoxue Liu,Zhiyao Chen,Shenhao Jiang,Lin Wang,Min Tao,Liyan Miao
Over the past decades, therapeutic drug monitoring (TDM) of tyrosine kinase inhibitors (TKIs) and their main active metabolites has shown benefits in improving treatment efficacy and safety. Therefore, a sensitive, simple and economical ultrahigh-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the determination of six oral tyrosine kinase inhibitors (TKIs) and two active metabolites, including imatinib (IMA), N-desmethyl imatinib (NDIMA), sunitinib (SUNI), N-desethyl sunitinib (NDSUNI), regorafenib (REGO), nilotinib (NILO), dasatinib (DASA) and osimertinib (OSI) in human plasma/serum for therapeutic drug monitoring. The plasma/serum samples were deproteinated with acetonitrile after spiking with two deuterated internal standards (ISs, [ 2 H 8 ]-imatinib and [ 2 H 10 ]-sunitinib) and separated on a 40 °C ACQUITY UPLC® BEH C 18 column (1.7 µm, 2.1 mm × 50 mm). The mobile phase was composed of acetonitrile (solution A) and water-formic acid-ammonium acetate (1 M) (994:1:5, v/v/v, solution B). Gradient elution was applied at a flow rate of 0.4 mL/min. Detection was carried out using a Triple Quad 5500 tandem mass spectrometer coupled with an electrospray ionization (ESI) source in positive mode. The method was validated over the calibration curve (CV) range of 2–400 ng/mL for NDSUNI and DASA, 2.5–500 ng/mL for SUNI, 10–2000 ng/mL NDIMA and OSI, 20–4000 ng/mL for NILO, 30–6000 ng/mL for REGO and 50–10000 ng/mL for IMA using linear regression and 1/x 2 weighting. No difference was observed in the matrix effect (ME) among blank human plasma, hemolytic plasma, lipemic plasma, plasma spiked with ten commonly used drugs by cancer patients, or serum samples in general. The standard curve fitted by two standard curves of serum and plasma showed good linearity, and the precision and accuracy results of QC samples in both plasma and serum were acceptable and the concentration was comparable. To provide a clinical reference for the operation, the stability of the whole process from sample collection to drug detection was verified. SUNI and NDSUNI showed obvious photoisomerization under light exposure. Therefore, strict light protection was applied for all sample collection and handling steps of SUNI and NDSUNI. Compared with heparin anticoagulant tubes, the stability of the eight compounds in both whole blood and plasma was better in K3-EDTA and sodium citrate anticoagulant tubes. Given that all the analytes were stable in plasma at 4 °C for 48 h and in whole blood at room temperature for 48 h but OSI and REGO were unstable in whole blood and plasma at room temperature, samples should be centrifuged as soon as possible to be preserved as plasma at 4 °C when OSI or REGO is detected. In conclusion, this validated method can provide support for clinical practice, such as therapeutic drug monitoring (TDM) and pharmacokinetic studies of these six TKIs and two active metabolites.
研究领域:
药理学
·
临床医学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2022
·
IF 6.911
Lin Li,Hongyu Zhang,Mengdan Zhang,Ting Wang,Xiaohong Hou
MIL-88B(Fe)/cellulose microspheres (MIL-88B(Fe)/CMs) were characterized by the means of SEM, XRD, TGA and N 2 adsorption-desorption test. The composite was used as the sorbent for fully automated dispersive pipette extraction (DPX), after introducing CMs as the support, the loss of MIL-88B(Fe) in DPX was avoided. Coupled to UPLC-MS/MS, the proposed method was employed for the analysis of trace sulfonamides (SAs) in milk samples. The parameters affecting the extraction efficiency, including pH of sample solution, the rate of aspiration and dispense, amount of the adsorbent, type and volume of elution solvent were optimized. Under the optimal conditions, good linearity (r ≥ 0.9978 for five analytes), high sensitivity (limit of detection: 0.00660–0.0136 μg kg −1 ) and satisfactory recovery (69.8%–100.9%) were achieved. Furthermore, the sorbent showed desirable reusability over eight extraction cycles. Compared with other methods for the pretreatment of SAs, the proposed method showed advantages of high sensitivity, less sorbent consumption, environmental friendliness and automation, providing a promising protocol for sample preparation.
研究领域:
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Frontiers in Pharmacology
·
2024
·
IF 4.4
Lan Tian,Duan Guozhen,Qi Youchao,Almezgagi Maged,Fan Guanghui,Ma Yonggui
Wolfberry, esteemed as a traditional Chinese medicinal material and functional food, is replete with nutrients and boasts a diverse array of health benefits, including hypoglycemic, antitumor, antioxidant, anti-inflammatory, and immune-enhancing properties. Notably, inflammation is a pivotal factor in the onset and progression of numerous diseases. Despite this, there is a paucity of research on the comprehensive evaluation of the components found in different wolfberries, and the exploration of their primary active components is limited. To address this issue, we conducted a comprehensive targeted metabolomics analysis, employing statistical methods such as principal component analysis (PCA), orthogonal partial least squares discriminant analysis (OPLS-DA), KEGG pathway analysis, and volcano plots to delineate the compositional differences among red, black, and yellow wolfberries. Furthermore, we investigated the anti-inflammatory effects of their primary components through in vitro experiments. Our analysis revealed a total of 1,104 chemical compositions in the three wolfberries, with alkaloids, phenolic acids, flavonoids, and lipids being the predominant nutritional components. KEGG enrichment analysis indicated that these compositions were primarily involved in the biosynthesis of secondary metabolites, ABC transport, and galactose metabolism pathway. Moreover, our study demonstrated that quercetin exhibited dose-dependent anti-inflammatory activity in LPS-stimulated HUVECs. It effectively inhibited the production of inflammatory factors such as TNF-α, MCP-1, and IL-1β, while also down-regulating the gene and protein expression levels of ICAM-1 and VCAM-1. In conclusion, our findings indicate that there are variations in compositions among the three wolfberries, with flavonoids being the most abundant, and in vitro studies also confirmed the anti-inflammatory potential of quercetin. It is worth noting that Lycium ruthenicum contains higher levels of antioxidant components and possesses greater nutritional value, providing valuable insights for the future development and utilization of the three wolfberries.
研究领域:
药理学
·
代谢组学
·
生物化学
·
药物化学
·
植物科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHIMICA ACTA
·
2017
·Vol. 184
·期 8
·2981-2990
·
IF 4.58
Wang Ting,Liu Siyu,Gao Guihua,Zhao Pan,Lu Nan,Lun Xiaowen,Hou Xiaohong
The authors describe a method for magnetic solid phase extraction (MSPE) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the quantitation of eight non-steroidal anti-inflammatory drugs (NSAIDs) in wastewater and environmental water samples. Specifically, the NSAIDs were directly extracted by using a magnetic nanocomposite of type Fe 3 O 4 /MIL-101(Cr) (Matérial Institute Lavoisier, MIL) from 50 mL water samples without any further cleanup. The effects of the amount of adsorbent, pH value, salt concentration, ultrasonic extraction time, desorption solvent nature and volume and desorption time were investigated. Under the optimal conditions, UPLC-MS/MS based detection resulted in the following figures of merit: (a) Linear calibration plots that typically extend from 0.1 (0.2, 0.05, 0.02) to 50 μg·L −1 , depending on the compound; (b) detection limits between 3 to 60 ng·L −1 ; and (c), recoveries varying from 81.2% to 116.8% with relative standard deviations between 0.4% and 10.8%. The adsorption of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was characterized by adsorption isotherms, kinetics and thermodynamics studies and provides a deeper insight into the adsorption mechanism. Compared to other method for pretreatment and preconcentration of NSAIDs, the new method is more rapid, sensitive, accurate and eco-friendly. The method was successfully applied to the determination of the NSAID residues in a variety of real environmental and wastewater samples.
Schematic of a method for determination of non-steroidal anti-inflammatory drugs (NSAIDs) in environmental water by magnetic solid phase extraction based on Fe 3 O 4 /MIL-101(Cr) combined with UPLC-MS/MS. The adsorption mechanism of NSAIDs on Fe 3 O 4 /MIL-101(Cr) was studied.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2022
·Vol. 30
·期 10
·27357-27371
·
IF 5.19
Ma Qing-guang,Wan Yi-ping,Liu Ze-hua,Dang Zhi
Analytical method for three natural estrogens (NEs) and their sulfate and glucuronide conjugates in waste and river waters using solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been available, but problems including poor recovery exist. In order to solve these, some optimizations have been performed in this work. For sample preparation, both rinse and elution solutions were optimized, in which 6 mL of MeOH/water (1:9, v/v), MeOH/Ace/water (10:2:88, v/v/v), and MeOH/NH 4 OH/water (10:2:88, v/v/v) were determined as the rinse solution, while 6 mL of 2.0% NH 4 OH/MeOH was determined as the elution solution for conjugated NEs (C-NEs). For mobile phase, addition of NH 4 F could obviously enhance the signal response of the nine target compounds, and the optimized addition concentration was 0.5 mmol/L. The developed efficient method was validated and showed excellent linearity for each target compound ( R 2 > 0.998), low limit of quantifications (LOQs, 0.07–1.29 ng/L) in four different water matrices, and excellent recovery efficiencies of 81.0–116.1% in influent, effluent, ultra-pure, and river water samples with low relative standard deviations (RSDs, 0.6–13.6%). The optimized method was successfully applied to influent, effluent, and Pearl River water, among which three NEs were all detected, while five C-NEs were found in the influent, three C-NEs were detected in the effluent, and two C-NEs were found in the Pearl River water, indicating the wide distribution of NEs and C-NEs in different water environments. This work provided a reliable and efficient analytical method for simultaneous trace determination of NEs and C-NEs, which had satisfactory absolute recoveries with low RSDs, low LOQs, and time-saving for both analysis and nitrogen drying.
研究领域:
环境科学
·
分析化学
·
水质
✓ 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）