Phosphatidylcholine (PC), a key phospholipid, contains 2 fatty acids that can be bound at the sn-1 and sn-2 positions, resulting in positional isomers when different fatty acids are attached. Currently, there is no established method for identifying phospholipid molecular species and quantifying individual isomers using authentic standards of each PC isomer. In this study, we prepare authentic analytical standards for PC positional isomers through chemical synthesis and preparative purification. These isomers contain docosahexaenoic acid (DHA, 22:6) and palmitic acid (16:0) attached at the sn-1 and sn-2 positions and are denoted as PC(22:6/16:0) and PC(16:0/22:6), respectively. Standard solutions of PC(22:6/16:0) and PC(16:0/22:6) were analyzed using liquid chromatography-tandem mass spectrometry, and calibration curves of the PC positional isomers were generated to compare their ionization efficiencies. The ionization efficiency of PC(22:6/16:0) was 2.32 times higher than that of PC(16:0/22:6), indicating that the ionization efficiency depends on the binding position of the fatty acid. Elucidating and correcting the differences in the ionization efficiencies of the PC positional isomers will enable the accurate quantitative analysis of lipidomes in the future.
磷脂酰胆碱（PC）是一种重要的磷脂，它含有两种脂肪酸，可分别结合在 sn-1 和 sn-2 位上，当连接不同的脂肪酸时会产生位置异构体。目前，还没有一种成熟的方法可以利用每种 PC 异构体的真品标准来鉴别磷脂分子种类和量化单个异构体。在本研究中，我们通过化学合成和制备纯化的方法制备了 PC 位置异构体的真实分析标准物质。这些异构体含有连接在 sn-1 和 sn-2 位置的二十二碳六烯酸（DHA，22:6）和棕榈酸（16:0），分别称为 PC(22:6/16:0) 和 PC(16:0/22:6)。采用液相色谱-串联质谱法分析了 PC(22:6/16:0) 和 PC(16:0/22:6) 的标准溶液，并绘制了 PC 位置异构体的校准曲线，以比较它们的电离效率。PC(22:6/16:0) 的电离效率是 PC(16:0/22:6) 的 2.32 倍，表明电离效率取决于脂肪酸的结合位置。阐明并纠正 PC 位置异构体电离效率的差异将有助于今后对脂质体进行精确的定量分析。
{"title":"Evaluation of the ionization efficiency in phosphatidylcholine positional isomers with docosahexaenoic acid bound to the sn-1 or sn-2 position","authors":"Kana Fujiwara , Seiya Tanaka , Koyama Tomoyuki , Kazuaki Yoshinaga , Naohiro Gotoh","doi":"10.1016/j.jchromb.2024.124355","DOIUrl":"10.1016/j.jchromb.2024.124355","url":null,"abstract":"<div><div>Phosphatidylcholine (PC), a key phospholipid, contains 2 fatty acids that can be bound at the sn-1 and sn-2 positions, resulting in positional isomers when different fatty acids are attached. Currently, there is no established method for identifying phospholipid molecular species and quantifying individual isomers using authentic standards of each PC isomer. In this study, we prepare authentic analytical standards for PC positional isomers through chemical synthesis and preparative purification. These isomers contain docosahexaenoic acid (DHA, 22:6) and palmitic acid (16:0) attached at the sn-1 and sn-2 positions and are denoted as PC(22:6/16:0) and PC(16:0/22:6), respectively. Standard solutions of PC(22:6/16:0) and PC(16:0/22:6) were analyzed using liquid chromatography-tandem mass spectrometry, and calibration curves of the PC positional isomers were generated to compare their ionization efficiencies. The ionization efficiency of PC(22:6/16:0) was 2.32 times higher than that of PC(16:0/22:6), indicating that the ionization efficiency depends on the binding position of the fatty acid. Elucidating and correcting the differences in the ionization efficiencies of the PC positional isomers will enable the accurate quantitative analysis of lipidomes in the future.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124355"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142643556","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-01DOI: 10.1016/j.jchromb.2024.124348
Jian Fei , Qiuyue Sha , Wenjie Zhu , Si Liu , Zhaoyu Hu , Wei Du , Xin Liu
Aliphatic amines are widely distributed in the environment and food sources, posing potential health risks through skin and mucosal irritation. Consequently, their quantitative detection is crucial for assessing environmental health. Despite high reactivity and fluorescence properties of succinimidyl ester-based derivatization reagents, their application in the aliphatic amines detection is hampered by challenges such as limited detection sensitivity and fluorescence interference. We established an innovative synthetic approach to produce a series of succinimidyl esters with the desirable substituents. This advancement enabled the creation of efficient and highly sensitive reagents for the detection of aliphatic amines. Among them, 2-methyl-6-methoxy-4-quinolinecarboxylic acid N-hydroxysuccinimide ester (MMQC-OSu) exhibited the best detection performance. MMQC-OSu reacted with aliphatic amines at 40 °C in pH 8.0 buffer for 20 min, which was subsequently separated in a C18 chromatographic column with the fluorescence detection wavelength of 336/432 nm. This detection approach featured a rapid and mild reaction process, minimal interference from corresponding hydrolysis products, and impressive sensitivity (0.05 nM). These characteristics indicate that MMQC-OSu significantly surpassing commercial aliphatic amines detection reagents. Finally, the detection strategy of MMQC-OSu was successfully applied in environmental sample analysis, with recovery rate of 93 %–108 % and RSDs between 1.4 % and 6.5 %.
{"title":"Synthesis of 2-methyl-6-methoxy-4-quinolinecarboxylic acid N-hydroxysuccinimide ester (MMQC-OSu) for streamlined and effective HPLC-based fluorescence detection of aliphatic amines in environmental samples","authors":"Jian Fei , Qiuyue Sha , Wenjie Zhu , Si Liu , Zhaoyu Hu , Wei Du , Xin Liu","doi":"10.1016/j.jchromb.2024.124348","DOIUrl":"10.1016/j.jchromb.2024.124348","url":null,"abstract":"<div><div>Aliphatic amines are widely distributed in the environment and food sources, posing potential health risks through skin and mucosal irritation. Consequently, their quantitative detection is crucial for assessing environmental health. Despite high reactivity and fluorescence properties of succinimidyl ester-based derivatization reagents, their application in the aliphatic amines detection is hampered by challenges such as limited detection sensitivity and fluorescence interference. We established an innovative synthetic approach to produce a series of succinimidyl esters with the desirable substituents. This advancement enabled the creation of efficient and highly sensitive reagents for the detection of aliphatic amines. Among them, 2-methyl-6-methoxy-4-quinolinecarboxylic acid N-hydroxysuccinimide ester (MMQC-OSu) exhibited the best detection performance. MMQC-OSu reacted with aliphatic amines at 40 °C in pH 8.0 buffer for 20 min, which was subsequently separated in a C18 chromatographic column with the fluorescence detection wavelength of 336/432 nm. This detection approach featured a rapid and mild reaction process, minimal interference from corresponding hydrolysis products, and impressive sensitivity (0.05 nM). These characteristics indicate that MMQC-OSu significantly surpassing commercial aliphatic amines detection reagents. Finally, the detection strategy of MMQC-OSu was successfully applied in environmental sample analysis, with recovery rate of 93 %–108 % and RSDs between 1.4 % and 6.5 %.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124348"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592594","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This study explores the application of imaged capillary isoelectric focusing (icIEF) to distinguish and quantify mispairing byproducts in asymmetric WuXiBody-based bispecific antibodies (AsWXbsAbs). Bispecific antibody (BsAb), developed using Knobs-into-Holes (KiH) technology, often result in byproducts such as knob-knob (KK) and hole-hole (HH) homodimers, which share similar sizes with the target BsAb, complicating their separation by traditional methods like size exclusion chromatography-high performance liquid chromatography (SEC-HPLC). Our approach leverages the unique pI differences introduced by substituting the CH1/CL domain with the T cell receptor (TCR) constant domain in AsWXbsAbs. This modification enables icIEF to effectively differentiate between the KK and HH homodimers and the target BsAb. Through the construction and expression of heavy and light chain variants, we validated that the experimental pI values aligned with theoretical predictions, confirming icIEF’s capability in distinguishing these entities. Enrichment of in-process K-related and H-related species was achieved, allowing for high-purity samples necessary for icIEF method development. The method was qualified and showed good specificity and linearity, with a quantitation limit of 4 % for K-related species (R2 = 0.9919) and 1 % for H-related species (R2 = 0.9805). This method was used effectively as an in-process test and release assay, proving its simple and quick utility in multiple AsWXbsAbs projects.
本研究探索了成像毛细管等电聚焦（icIEF）技术在基于不对称乌希抗体的双特异性抗体（AsWXbsAbs）中的应用，以区分和量化配对错误的副产物。使用Knobs-into-Holes（KiH）技术开发的双特异性抗体（BsAb）通常会产生副产物，如与目标BsAb大小相似的knob-knob（KK）和hole-hole（HH）同源二聚体，从而使传统的尺寸排阻色谱-高效液相色谱（SEC-HPLC）等方法分离它们变得复杂。我们的方法利用了 AsWXbsAbs 中用 T 细胞受体（TCR）恒定结构域取代 CH1/CL 结构域所带来的独特 pI 差异。这种修改使 icIEF 能够有效区分 KK 和 HH 同源二聚体和目标 BsAb。通过构建和表达重链和轻链变体，我们验证了实验 pI 值与理论预测值一致，证实了 icIEF 区分这些实体的能力。我们实现了过程中 K 相关和 H 相关物种的富集，从而获得了开发 icIEF 方法所需的高纯度样本。经鉴定，该方法具有良好的特异性和线性，K 相关物种的定量限为 4%（R2 = 0.9919），H 相关物种的定量限为 1%（R2 = 0.9805）。该方法被有效地用作过程中测试和释放检测，证明了其在多个 AsWXbsAbs 项目中简单快捷的实用性。
{"title":"Development of imaged capillary isoelectric focusing as a platform mispairing byproduct testing method for asymmetric WuXiBody-based bispecific antibodies","authors":"Liping Zhan , Luping Xie , Fujiao Lv , Jincui Huang , Zhi Jian Chen , Li Wang , Zhiqiang Chen","doi":"10.1016/j.jchromb.2024.124357","DOIUrl":"10.1016/j.jchromb.2024.124357","url":null,"abstract":"<div><div>This study explores the application of imaged capillary isoelectric focusing (icIEF) to distinguish and quantify mispairing byproducts in asymmetric WuXiBody-based bispecific antibodies (AsWXbsAbs). Bispecific antibody (BsAb), developed using Knobs-into-Holes (KiH) technology, often result in byproducts such as knob-knob (KK) and hole-hole (HH) homodimers, which share similar sizes with the target BsAb, complicating their separation by traditional methods like size exclusion chromatography-high performance liquid chromatography (SEC-HPLC). Our approach leverages the unique pI differences introduced by substituting the CH1/CL domain with the T cell receptor (TCR) constant domain in AsWXbsAbs. This modification enables icIEF to effectively differentiate between the KK and HH homodimers and the target BsAb. Through the construction and expression of heavy and light chain variants, we validated that the experimental pI values aligned with theoretical predictions, confirming icIEF’s capability in distinguishing these entities. Enrichment of in-process K-related and H-related species was achieved, allowing for high-purity samples necessary for icIEF method development. The method was qualified and showed good specificity and linearity, with a quantitation limit of 4 % for K-related species (R<sup>2</sup> = 0.9919) and 1 % for H-related species (R<sup>2</sup> = 0.9805). This method was used effectively as an in-process test and release assay, proving its simple and quick utility in multiple AsWXbsAbs projects.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124357"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142586149","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-01DOI: 10.1016/j.jchromb.2024.124342
Jordan I. Oliver, Antony N. Davies, Richard Dinsdale
This study has developed a new targeted methodology for the separation, detection, and quantification of metabolites from the wider energy metabolome of industrially important microorganisms such as Saccharomyces cerevisiae in a single analytical sample. This has been achieved using UHPLC-MS technology in HILIC mode. Absolute concentrations of metabolites nicotinamide adenine dinucleotide (NAD), nicotinamide adenine dinucleotide reduced (NADH), nicotinamide adenine dinucleotide phosphate (NADP), nicotinamide adenine dinucleotide phosphate reduced (NADPH), flavin adenine dinucleotide (FAD), adenosine-monophosphate (AMP), adenosine-diphosphate (ADP), and adenosine-triphosphate (ATP) were determined in a single extraction and analytical methodology.
This study demonstrated the development of a rapid, statistically robust, and reproducible methodology through regression calibrations of standard samples from 0.1 to 100 µMol providing a correlation value of r2 = >0.98 for all metabolites. Sample preparation, extraction and analytical methodologies used showed high accuracy, sensitivity, and recovery. With an LOD and LOQ for the targeted analysis of metabolites from the wider energy metabolism in a single sample and analytical run with the lowest LOD of 0.055 nMol (±0.002) and lowest LOQ of 0.167 nMol (±0.006). This method was then applied to Saccharomyces cerevisiae cell culture to evaluate the methodology in industrially used microbial cultures. Results obtained have been statistically determined to be robust and reproducible through recovery analysis using deuterated and isotopically labelled internal standards AMP-15N, ADP-15N and ATP-d14.
{"title":"Quantifying the extended energy metabolome of industrially important microorganisms (Saccharomyces cerevisiae) using ultra-performance liquid chromatography with mass spectrometry","authors":"Jordan I. Oliver, Antony N. Davies, Richard Dinsdale","doi":"10.1016/j.jchromb.2024.124342","DOIUrl":"10.1016/j.jchromb.2024.124342","url":null,"abstract":"<div><div>This study has developed a new targeted methodology for the separation, detection, and quantification of metabolites from the wider energy metabolome of industrially important microorganisms such as <em>Saccharomyces cerevisiae</em> in a single analytical sample. This has been achieved using UHPLC-MS technology in HILIC mode. Absolute concentrations of metabolites nicotinamide adenine dinucleotide (NAD), nicotinamide adenine dinucleotide reduced (NADH), nicotinamide adenine dinucleotide phosphate (NADP), nicotinamide adenine dinucleotide phosphate reduced (NADPH), flavin adenine dinucleotide (FAD), adenosine-monophosphate (AMP), adenosine-diphosphate (ADP), and adenosine-triphosphate (ATP) were determined in a single extraction and analytical methodology.</div><div>This study demonstrated the development of a rapid, statistically robust, and reproducible methodology through regression calibrations of standard samples from 0.1 to 100 µMol providing a correlation value of r<sup>2</sup> = >0.98 for all metabolites. Sample preparation, extraction and analytical methodologies used showed high accuracy, sensitivity, and recovery. With an LOD and LOQ for the targeted analysis of metabolites from the wider energy metabolism in a single sample and analytical run with the lowest LOD of 0.055 nMol (±0.002) and lowest LOQ of 0.167 nMol (±0.006). This method was then applied to <em>Saccharomyces cerevisiae</em> cell culture to evaluate the methodology in industrially used microbial cultures. Results obtained have been statistically determined to be robust and reproducible through recovery analysis using deuterated and isotopically labelled internal standards AMP-<sup>15</sup>N, ADP-<sup>15</sup>N and ATP-d<sub>14</sub>.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124342"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142560707","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-01DOI: 10.1016/j.jchromb.2024.124358
Kexin Lin , Lijuan Xiong , Wen Zhang , Xuan Chen , Jieqi Zhu , Xiaofei Li , Jianyong Zhang
Cisplatin (CP) is a widely utilized anticancer drug, which also produces significant side effects, notably acute kidney injury (AKI). Fermented Eucommia ulmoides leaf (FEUL), a medicinal and edible Chinese herbal remedy, is known for its renoprotective properties. However, the effect and underlying mechanism of FEUL extract in AKI therapy have remained largely unexplored. This research aimed to elucidate the protective roles of FEUL extract in an AKI mouse model through biochemical assays, histopathological examinations, and investigating the underlying mechanisms based on metabolomics and network pharmacology. The findings demonstrated that pretreatment with orally administered FEUL extract significantly reduced blood urea nitrogen (BUN), and serum creatinine (SCr) levels, and ameliorated CP-induced kidney histopathological injuries. Moreover, FEUL extract attenuated CP-induced endoplasmic reticulum (ER) stress by reducing the protein expressions of PERK, IRE 1α, GRP78, ATF6, ATF4, and CHOP. The metabolomics results indicated that a total of 31 metabolites, involved in taurine and hypotaurine metabolism, lysine degradation, and steroid hormone biosynthesis, were altered after FEUL extract administration. Furthermore, metabolomics integrated with network pharmacology revealed that 8 targets, 4 metabolites, and 3 key pathways including steroid hormone biosynthesis, purine metabolism, and tryptophan metabolism were the main mechanisms of FEUL extract in treating CP-induced AKI. These findings suggested that FEUL extract could offer valuable insights for potential CP-induced AKI treatment strategies.
顺铂（CP）是一种广泛使用的抗癌药物，也会产生严重的副作用，尤其是急性肾损伤（AKI）。发酵杜仲叶（FEUL）是一种药用和食用中草药，以其肾脏保护特性而闻名。然而，发酵杜仲叶提取物在 AKI 治疗中的作用和内在机制在很大程度上仍未得到探索。本研究旨在通过生化检测、组织病理学检查以及基于代谢组学和网络药理学的潜在机制研究，阐明鱼腥草提取物在 AKI 小鼠模型中的保护作用。研究结果表明，口服 FEUL 提取物可显著降低血尿素氮（BUN）和血清肌酐（SCr）水平，并改善 CP 诱导的肾脏组织病理学损伤。此外，FEUL提取物还能降低PERK、IRE 1α、GRP78、ATF6、ATF4和CHOP的蛋白表达，从而减轻CP诱导的内质网（ER）应激。代谢组学研究结果表明，服用 FEUL 提取物后，参与牛磺酸和低牛磺酸代谢、赖氨酸降解和类固醇激素生物合成的 31 种代谢物发生了变化。此外，代谢组学与网络药理学相结合发现，8个靶点、4个代谢物和3个关键通路（包括类固醇激素生物合成、嘌呤代谢和色氨酸代谢）是FEUL提取物治疗CP诱导的AKI的主要机制。这些研究结果表明，鱼腥草提取物可为潜在的CP诱导的AKI治疗策略提供有价值的见解。
{"title":"Exploring the pharmacological mechanism of fermented Eucommia ulmoides leaf extract in the treatment of cisplatin-induced kidney injury in mice: Integrated traditional pharmacology, metabolomics and network pharmacology","authors":"Kexin Lin , Lijuan Xiong , Wen Zhang , Xuan Chen , Jieqi Zhu , Xiaofei Li , Jianyong Zhang","doi":"10.1016/j.jchromb.2024.124358","DOIUrl":"10.1016/j.jchromb.2024.124358","url":null,"abstract":"<div><div>Cisplatin (CP) is a widely utilized anticancer drug, which also produces significant side effects, notably acute kidney injury (AKI). Fermented <em>Eucommia ulmoides</em> leaf (FEUL), a medicinal and edible Chinese herbal remedy, is known for its renoprotective properties. However, the effect and underlying mechanism of FEUL extract in AKI therapy have remained largely unexplored. This research aimed to elucidate the protective roles of FEUL extract in an AKI mouse model through biochemical assays, histopathological examinations, and investigating the underlying mechanisms based on metabolomics and network pharmacology. The findings demonstrated that pretreatment with orally administered FEUL extract significantly reduced blood urea nitrogen (BUN), and serum creatinine (SCr) levels, and ameliorated CP-induced kidney histopathological injuries. Moreover, FEUL extract attenuated CP-induced endoplasmic reticulum (ER) stress by reducing the protein expressions of PERK, IRE 1α, GRP78, ATF6, ATF4, and CHOP. The metabolomics results indicated that a total of 31 metabolites, involved in taurine and hypotaurine metabolism, lysine degradation, and steroid hormone biosynthesis, were altered after FEUL extract administration. Furthermore, metabolomics integrated with network pharmacology revealed that 8 targets, 4 metabolites, and 3 key pathways including steroid hormone biosynthesis, purine metabolism, and tryptophan metabolism were the main mechanisms of FEUL extract in treating CP-induced AKI. These findings suggested that FEUL extract could offer valuable insights for potential CP-induced AKI treatment strategies.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124358"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611284","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bletilla striata is a perennial herb that was first published in Shennong’s Classic of the Materia Medica, pharmacological studies have shown that it has the activities of promoting wound healing, anti-inflammatory and antioxidant. However, the relationship between the antioxidant activity and the chemical composition of Bletilla striata is still unclear. In this paper, the chemometric method was used to construct the spectral effect relationship between the fingerprints of 20 batches of Bletilla striata extracts from different origins and their in vitro antioxidant activities. The results showed that the chemical composition of the samples from different sources varied significantly, while the samples from Shaanxi and Hubei provinces were of relatively better quality. Among the 10 common peaks, coelonin, gymnoside IX and dactylorhin A were considered to be significantly correlated with the antioxidant activity of Bletilla striata. The results of this study will provide a basis and further insights for the quality evaluation and quality control of Bletilla striata.
白芨是一种多年生草本植物，最早见于《神农本草经》，药理研究表明它具有促进伤口愈合、抗炎和抗氧化的活性。然而，抗氧化活性与白芨化学成分之间的关系尚不明确。本文采用化学计量学方法构建了20批次不同产地的条叶紫苏提取物指纹图谱与其体外抗氧化活性之间的谱效关系。结果表明，不同产地样品的化学成分差异较大，陕西省和湖北省的样品质量相对较好。在 10 个常见峰值中，认为薏苡仁苷、钩藤苷 IX 和麦冬皂苷 A 与条纹叶紫苏的抗氧化活性显著相关。本研究的结果将为条斑紫苏的质量评价和质量控制提供依据和进一步的见解。
{"title":"Spectrum-effect relationship between HPLC fingerprints and antioxidant activities of Bletilla striata","authors":"Sha Wen, Yuzhi Luo, Lingyi Liu, Lili Zhou, Lingli Li, Siqi Wang, Huixin Song, Songyuan Xia, Weifeng Li, Xiaofeng Niu","doi":"10.1016/j.jchromb.2024.124351","DOIUrl":"10.1016/j.jchromb.2024.124351","url":null,"abstract":"<div><div><em>Bletilla striata</em> is a perennial herb that was first published in Shennong’s Classic of the Materia Medica, pharmacological studies have shown that it has the activities of promoting wound healing, anti-inflammatory and antioxidant. However, the relationship between the antioxidant activity and the chemical composition of <em>Bletilla striata</em> is still unclear. In this paper, the chemometric method was used to construct the spectral effect relationship between the fingerprints of 20 batches of <em>Bletilla striata</em> extracts from different origins and their in vitro antioxidant activities. The results showed that the chemical composition of the samples from different sources varied significantly, while the samples from Shaanxi and Hubei provinces were of relatively better quality. Among the 10 common peaks, coelonin, gymnoside IX and dactylorhin A were considered to be significantly correlated with the antioxidant activity of <em>Bletilla striata</em>. The results of this study will provide a basis and further insights for the quality evaluation and quality control of <em>Bletilla striata.</em></div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124351"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142638172","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-01DOI: 10.1016/j.jchromb.2024.124354
Zvonimir Mlinarić
An article by Harsha Shi et al. raises multiple concerns regarding sample preparation, the presence of the analyte in the analyzed solution, authenticity of the MS spectra, administration of drugs and blood collection, choice of internal standard, obtained pharmacokinetic parameters and usage of chromatographic column and solvents. While the research topic is interesting and the development of bioanalytical methods for novel drugs is crucial, this article does not seem to meet the analytical and methodological standards for the reliable determination of adagrasib and pembrolizumab in plasma samples. A detailed explanation is given in the letter.
Harsha Shi 等人的一篇文章提出了样品制备、分析溶液中分析物的存在、质谱的真实性、给药和采血、内标的选择、获得的药代动力学参数以及色谱柱和溶剂的使用等多方面的问题。虽然研究课题很有意义，开发新型药物的生物分析方法也很关键，但这篇文章似乎不符合可靠测定血浆样本中阿达拉昔布和彭博利珠单抗的分析和方法学标准。信中给出了详细解释。
{"title":"Limitations in LC-MS/MS application for adagrasib and pembrolizumab quantification in rat plasma","authors":"Zvonimir Mlinarić","doi":"10.1016/j.jchromb.2024.124354","DOIUrl":"10.1016/j.jchromb.2024.124354","url":null,"abstract":"<div><div>An article by Harsha Shi et al. raises multiple concerns regarding sample preparation, the presence of the analyte in the analyzed solution, authenticity of the MS spectra, administration of drugs and blood collection, choice of internal standard, obtained pharmacokinetic parameters and usage of chromatographic column and solvents. While the research topic is interesting and the development of bioanalytical methods for novel drugs is crucial, this article does not seem to meet the analytical and methodological standards for the reliable determination of adagrasib and pembrolizumab in plasma samples. A detailed explanation is given in the letter.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124354"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611288","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-11-01DOI: 10.1016/j.jchromb.2024.124356
Yang Zhou , Pu Wang , Zuying Zhou , Meng Zhou , Mingyan Chi , Lin Zheng , Yong Huang
Biancaea decapetala (Roth) O.Deg. (Fabaceae), traditionally utilized by the Hmong for treating rheumatoid arthritis (RA), has its pharmacokinetic behavior under disease conditions largely unexplored. In view of this, a UPLC-MS/MS method was established for the determination of protosappanin B (PTB), protosappanin B-3-O-β-D-glucoside (PTD), and 3-deoxysappanchalcone (3-DSC), key bioactive components of the herb, in rat plasma and RAW264.7 cells to explore the effect of disease state on the pharmacokinetic profiles changes of these three components in vitro and in vivo. These components were detected using multiple reaction monitoring (MRM) process in positive and negative mode. Each calibration curve had a high R2 value of > 0.99. The intra- and inter-day precisions of PTD, PTB, 3-DSC were all < 15 %, and accuracy ranged from 85 % to 115 %. The RSD values pertaining to stability, recovery, matrix effect, and stability remained below 15.0 %. It was successfully applied for the investigation of the pharmacokinetics of these three components in rat plasma and RAW264.7 cells after administration of Biancaea decapetala extracts (BDE). In rat pharmacokinetic experiments, significant differences were observed in the AUC(0-t), MRT(0-t), and Clz/F values of PTD, PTB, 3-DSC between adjuvant-induced arthritis (AA) and normal rats. In cellular pharmacokinetic experiments, comparison with the normal group revealed increased AUC(0-t) and MRT(0-t) for these three components in the LPS-induced inflammatory cell model, along with decreased Clz/F, which was consistent with in vivo experimental outcomes. These findings suggest an increased absorption rate and a decreased elimination rate of the three components of BDE in AA rats and inflammatory cells, indicating a potential alteration in the rate and extent of drug metabolism. This study provided a theoretical reference for further clarification of its pharmacodynamic basis.
{"title":"Quantitative analysis of three bioactive components of Biancaea decapetala extracts in rat plasma and RAW264.7 cells using UPLC-MS/MS and its application to comparative pharmacokinetics in normal and diseased states","authors":"Yang Zhou , Pu Wang , Zuying Zhou , Meng Zhou , Mingyan Chi , Lin Zheng , Yong Huang","doi":"10.1016/j.jchromb.2024.124356","DOIUrl":"10.1016/j.jchromb.2024.124356","url":null,"abstract":"<div><div><em>Biancaea decapetala</em> (Roth) O.Deg. (Fabaceae), traditionally utilized by the Hmong for treating rheumatoid arthritis (RA), has its pharmacokinetic behavior under disease conditions largely unexplored. In view of this, a UPLC-MS/MS method was established for the determination of protosappanin B (PTB), protosappanin B-3-<em>O-β-D</em>-glucoside (PTD), and 3-deoxysappanchalcone (3-DSC), key bioactive components of the herb, in rat plasma and RAW264.7 cells to explore the effect of disease state on the pharmacokinetic profiles changes of these three components <em>in vitro</em> and <em>in vivo</em>. These components were detected using multiple reaction monitoring (MRM) process in positive and negative mode. Each calibration curve had a high <em>R</em><sup>2</sup> value of > 0.99. The intra- and inter-day precisions of PTD, PTB, 3-DSC were all < 15 %, and accuracy ranged from 85 % to 115 %. The RSD values pertaining to stability, recovery, matrix effect, and stability remained below 15.0 %. It was successfully applied for the investigation of the pharmacokinetics of these three components in rat plasma and RAW264.7 cells after administration of <em>Biancaea decapetala</em> extracts (BDE). In rat pharmacokinetic experiments, significant differences were observed in the AUC<sub>(0-t)</sub>, MRT<sub>(0-t)</sub>, and <em>Cl</em><sub>z</sub>/<em>F</em> values of PTD, PTB, 3-DSC between adjuvant-induced arthritis (AA) and normal rats. In cellular pharmacokinetic experiments, comparison with the normal group revealed increased AUC<sub>(0-t)</sub> and MRT<sub>(0-t)</sub> for these three components in the LPS-induced inflammatory cell model, along with decreased <em>Cl</em><sub>z</sub>/<em>F</em>, which was consistent with <em>in vivo</em> experimental outcomes. These findings suggest an increased absorption rate and a decreased elimination rate of the three components of BDE in AA rats and inflammatory cells, indicating a potential alteration in the rate and extent of drug metabolism. This study provided a theoretical reference for further clarification of its pharmacodynamic basis.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1248 ","pages":"Article 124356"},"PeriodicalIF":2.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592621","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-15DOI: 10.1016/j.jchromb.2024.124343
Luyao Yu , Xiaoqian Chen , Yingxia Guo , Jiansong You , Meiyun Shi , Yalin Xi , Lei Yin
An ultra-high performance liquid chromatography tandem mass spectrometry cubed (UHPLC/MS3) assay coupled with protein precipitation and counter-extraction for detection of tricyclic glycopeptide vancomycin in human plasma was established and validated in this study. After protein precipitation and counter-extraction with dichloromethane, chromatographic separation of vancomycin and norvancomycin were performed on a reversed phase column (XBridge Peptide BEH C18 column, 2.1 × 100 mm I.D, 3.5 μm). The transition (parent ions → fragment ions → further fragment ions) at m/z 725.3 → 144.1 → 100.1 was used for quantification of vancomycin. The transition (parent ions → fragment ions) at m/z 718.3 → 144.2 was used for detection of norvancomycin. The linear range of the developed analytical method for quantification of vancomycin was 0.5–100 µg/mL (r = 0.9989). The range of intra- and inter-day precisions of the assay among low, medium and high concentrations is between 1.88 % and 6.33 %. The sensitivity of the analytical method was significantly improved by using MS3 technique as monitoring mode and counter-extraction with dichloromethane followed by protein precipitation as sample processing assay. The developed UHPLC/MS3 assay was successfully applied for clinical therapeutic drug monitoring (TDM) of vancomycin in 45 human plasma samples.
{"title":"Quantification of tricyclic glycopeptide in human plasma by UHPLC-MS3 coupled with counter-extraction follow by protein precipitation to enhance sensitivity","authors":"Luyao Yu , Xiaoqian Chen , Yingxia Guo , Jiansong You , Meiyun Shi , Yalin Xi , Lei Yin","doi":"10.1016/j.jchromb.2024.124343","DOIUrl":"10.1016/j.jchromb.2024.124343","url":null,"abstract":"<div><div>An ultra-high performance liquid chromatography tandem mass spectrometry cubed (UHPLC/MS<sup>3</sup>) assay coupled with protein precipitation and counter-extraction for detection of tricyclic glycopeptide vancomycin in human plasma was established and validated in this study. After protein precipitation and counter-extraction with dichloromethane, chromatographic separation of vancomycin and norvancomycin were performed on a reversed phase column (XBridge Peptide BEH C<sub>18</sub> column, 2.1 × 100 mm I.D, 3.5 μm). The transition (parent ions → fragment ions → further fragment ions) at <em>m</em>/<em>z</em> 725.3 → 144.1 → 100.1 was used for quantification of vancomycin. The transition (parent ions → fragment ions) at <em>m</em>/<em>z</em> 718.3 → 144.2 was used for detection of norvancomycin. The linear range of the developed analytical method for quantification of vancomycin was 0.5–100 µg/mL (r = 0.9989). The range of intra- and inter-day precisions of the assay among low, medium and high concentrations is between 1.88 % and 6.33 %. The sensitivity of the analytical method was significantly improved by using MS<sup>3</sup> technique as monitoring mode and counter-extraction with dichloromethane followed by protein precipitation as sample processing assay. The developed UHPLC/MS<sup>3</sup> assay was successfully applied for clinical therapeutic drug monitoring (TDM) of vancomycin in 45 human plasma samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124343"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142492172","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2024-10-15DOI: 10.1016/j.jchromb.2024.124338
Shuaibin Wu
In this study, a novel surface covalent reaction method was used to modify attapulgite nanoparticles on the surface of polypropylene adsorption membrane to adsorb various small molecular pollutants for the first time. The surface covalent reaction method has the advantage of step control. Therefore, the uniformity and stability of attapulgite nanoparticles can be ensured, and then could effectively improve the adsorption performance of polypropylene adsorption membrane. On the other hand, compared with various materials modified on the surface of polypropylene adsorption membrane currently, attapulgite nanoparticles has the characteristics of low cost and environmental friendliness, which is more conducive to the large-scale practical application. The polypropylene adsorption membrane modified with attapulgite nanoparticles was characterized by field emission scanning electron microscopy, fourier transform infrared spectrometer and X-ray diffractograph, and it was confirmed that the attapulgite nanoparticles was successfully modified on the surface of the polypropylene adsorption membrane. The experimental results showed that the adsorption capacities of polypropylene adsorption membrane modified with attapulgite nanoparticles could reach 11.53 mg/g, 8.7 mg/g and 5.78 mg/g for cyromazine, malachite green and dagenan respectively within 10 s. In the case of the above three analytes, the minimum detected concentration could reach 0.02 mg/mL, and the relative standard deviation was about 10 %. At the same time, the adsorption performance of polypropylene adsorption membrane modified with attapulgite nanoparticles did not decrease significantly after 50 cycles. A standard recovery of 76.8 % − 89.5 % and a relative standard deviation of 7.2 % − 15.2 % were obtained by using the polypropylene adsorption membrane modified with attapulgite nanoparticles to adsorb cyromazine in cucumber skin samples, indicating that the polypropylene adsorption membrane modified with attapulgite nanoparticles has the ability to treat complex samples.
{"title":"Preparation of attapulgite nanoparticles modified polypropylene adsorption membrane and its application in small molecular pollutant adsorption","authors":"Shuaibin Wu","doi":"10.1016/j.jchromb.2024.124338","DOIUrl":"10.1016/j.jchromb.2024.124338","url":null,"abstract":"<div><div>In this study, a novel surface covalent reaction method was used to modify attapulgite nanoparticles on the surface of polypropylene adsorption membrane to adsorb various small molecular pollutants for the first time. The surface covalent reaction method has the advantage of step control. Therefore, the uniformity and stability of attapulgite nanoparticles can be ensured, and then could effectively improve the adsorption performance of polypropylene adsorption membrane. On the other hand, compared with various materials modified on the surface of polypropylene adsorption membrane currently, attapulgite nanoparticles has the characteristics of low cost and environmental friendliness, which is more conducive to the large-scale practical application. The polypropylene adsorption membrane modified with attapulgite nanoparticles was characterized by field emission scanning electron microscopy, fourier transform infrared spectrometer and X-ray diffractograph, and it was confirmed that the attapulgite nanoparticles was successfully modified on the surface of the polypropylene adsorption membrane. The experimental results showed that the adsorption capacities of polypropylene adsorption membrane modified with attapulgite nanoparticles could reach 11.53 mg/g, 8.7 mg/g and 5.78 mg/g for cyromazine, malachite green and dagenan respectively within 10 s. In the case of the above three analytes, the minimum detected concentration could reach 0.02 mg/mL, and the relative standard deviation was about 10 %. At the same time, the adsorption performance of polypropylene adsorption membrane modified with attapulgite nanoparticles did not decrease significantly after 50 cycles. A standard recovery of 76.8 % − 89.5 % and a relative standard deviation of 7.2 % − 15.2 % were obtained by using the polypropylene adsorption membrane modified with attapulgite nanoparticles to adsorb cyromazine in cucumber skin samples, indicating that the polypropylene adsorption membrane modified with attapulgite nanoparticles has the ability to treat complex samples.</div></div>","PeriodicalId":348,"journal":{"name":"Journal of Chromatography B","volume":"1247 ","pages":"Article 124338"},"PeriodicalIF":2.8,"publicationDate":"2024-10-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142441917","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"医学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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