Journal of Chromatography A最新文献_第2页

Ultra-high pressure slalom chromatography: Application to the characterization of large DNA and RNA samples relevant in cell and gene therapy 超高压回旋色谱法：应用于细胞和基因治疗相关的大量 DNA 和 RNA 样品的表征。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-07 DOI: 10.1016/j.chroma.2024.465487

Fabrice Gritti

Slalom chromatography (SC), initially co-discovered by Boyes and Kasai in the late 1980s, has recently re-emerged as a breakthrough technique to rapidly analyze DNA samples. With the development of cutting-edge ultra-high pressure liquid chromatography (UHPLC) systems and columns, SC now offers enhanced resolution and sensitivity for analyzing large DNA samples. By revisiting the fundamentals of the SC retention mechanism (non-equilibrium separation mode) and considering the physicochemical properties of DNA biopolymers (contour length, extension under shear flow, relaxation time), we provide analytical chemists with a general strategy and framework for selecting the most relevant applications in the expanding field of cell and gene therapy. We then present proof-of-concept data demonstrating the rapid separation (under 2 min) of plasmid digest samples containing linear double-stranded (ds) DNA macromolecules starting from 2 kbp to 25 kbp, as well as the accurate size determination (

\pm

6%) of linear dsDNAs. Additionally, we show rapid baseline separation and quantification of extensible linear dsDNAs, along with the more rigid plasmid dsDNA (supercoiled/circular/nicked circular). We also quantify dsRNA impurities present in vitro transcription (IVT) media used for producing new mRNA therapeutics and assess dsRNA structural heterogeneity (conformational isomers). These findings aim to support in a near future application chemists in addressing emerging bioanalytical challenges in cell and gene therapy by offering advanced SC columns and methods.

回旋色谱法（SC）最初是由 Boyes 和 Kasai 在 20 世纪 80 年代末共同发现的，最近再次成为快速分析 DNA 样品的突破性技术。随着最先进的超高压液相色谱（UHPLC）系统和色谱柱的发展，SC 现可为分析大量 DNA 样品提供更高的分辨率和灵敏度。通过重新审视 SC 保留机制（非平衡分离模式）的基本原理，并考虑 DNA 生物聚合物的理化特性（轮廓长度、剪切流下的延伸、弛豫时间），我们为分析化学家提供了在不断扩大的细胞和基因治疗领域选择最相关应用的一般策略和框架。然后，我们展示了概念验证数据，这些数据证明了能快速分离（不到 2 分钟）含有线性双链 (ds) DNA 大分子的质粒消化样本（从 2 kbp 到 25 kbp），并能准确测定线性 dsDNA 的大小（±6%）。此外，我们还展示了快速基线分离和量化可延伸线性dsDNA以及刚性较强的质粒dsDNA（超卷曲/环状/挑刺环状）的方法。我们还量化了用于生产新型 mRNA 疗法的体外转录 (IVT) 培养基中的 dsRNA 杂质，并评估了 dsRNA 的结构异质性（构象异构体）。这些发现旨在通过提供先进的 SC 色谱柱和方法，帮助应用化学家在不久的将来应对细胞和基因治疗领域新出现的生物分析挑战。

{"title":"Ultra-high pressure slalom chromatography: Application to the characterization of large DNA and RNA samples relevant in cell and gene therapy","authors":"Fabrice Gritti","doi":"10.1016/j.chroma.2024.465487","DOIUrl":"10.1016/j.chroma.2024.465487","url":null,"abstract":"<div><div>Slalom chromatography (SC), initially co-discovered by Boyes and Kasai in the late 1980s, has recently re-emerged as a breakthrough technique to rapidly analyze DNA samples. With the development of cutting-edge ultra-high pressure liquid chromatography (UHPLC) systems and columns, SC now offers enhanced resolution and sensitivity for analyzing large DNA samples. By revisiting the fundamentals of the SC retention mechanism (non-equilibrium separation mode) and considering the physicochemical properties of DNA biopolymers (contour length, extension under shear flow, relaxation time), we provide analytical chemists with a general strategy and framework for selecting the most relevant applications in the expanding field of cell and gene therapy. We then present proof-of-concept data demonstrating the rapid separation (under 2 min) of plasmid digest samples containing linear double-stranded (ds) DNA macromolecules starting from 2 kbp to 25 kbp, as well as the accurate size determination (<span><math><mo>±</mo></math></span>6%) of linear dsDNAs. Additionally, we show rapid baseline separation and quantification of extensible linear dsDNAs, along with the more rigid plasmid dsDNA (supercoiled/circular/nicked circular). We also quantify dsRNA impurities present in vitro transcription (IVT) media used for producing new mRNA therapeutics and assess dsRNA structural heterogeneity (conformational isomers). These findings aim to support in a near future application chemists in addressing emerging bioanalytical challenges in cell and gene therapy by offering advanced SC columns and methods.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465487"},"PeriodicalIF":3.8,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611167","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Method development and comprehensive study of matrix effects for the determination of trace organic contaminants in lake sediments 用于测定湖泊沉积物中痕量有机污染物的方法开发和基质效应综合研究。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-06 DOI: 10.1016/j.chroma.2024.465504

François-Xavier Teysseire , Hubert Cabana , Pedro A. Segura

The presence of trace organic contaminants (TrOCs), such as pharmaceuticals, personal care products, additives, and polar pesticides in sediments of rivers and lakes highly impacted by anthropogenic activities makes sediments a secondary source of contamination for aquatic ecosystems. Considering this, a method for analyzing 44 TrOCs of diverse nature (including five transformation products, 13 pharmaceuticals, five personal care products, 14 pesticides, and seven additives) was developed and validated. It is based on extraction by pressurized liquid extraction (PLE), followed by purification and pre-concentration by solid phase extraction (SPE) and quantification by liquid chromatography coupled to a triple quadrupole mass spectrometer (LC-QqQMS). The method was optimized according to dispersant type, temperature, and extraction solvent. The influence of organic matter in sediments on quantitative analysis was also investigated in detail. Matrix effects were highly and significantly correlated (r=-0.9146, p < 0.0001) with retention time. Using internal standards showed the best results for effectively correcting matrix effects without affecting method sensitivity. The method was then validated according to key figures of merit: linearity (R² > 0.990), extraction recoveries (> 60 % for 34 compounds), trueness (bias % < 15 %), precision (relative standard deviation < 20 %) and matrix effects (between -13.3 % and 17.8 %). This method can be applied for routine analysis of TrOCs in different sediment matrices. The method was applied to ten lake sediment samples collected in Québec, Canada. Results demonstrated the presence of 17 compounds in at least one lake at concentrations between 0.07 to 1531 ng g^-1. The reported concentrations provide a first picture of the occurrence of chemical stressors in sediments of small lake highly anthropized ecosystems in Eastern Canada.

受人为活动影响较大的河流和湖泊的沉积物中存在痕量有机污染物（TrOCs），如药物、个人护理产品、添加剂和极性杀虫剂，这使得沉积物成为水生生态系统的二次污染源。有鉴于此，我们开发并验证了一种用于分析 44 种不同性质的 TrOCs（包括 5 种转化产品、13 种药物、5 种个人护理产品、14 种杀虫剂和 7 种添加剂）的方法。该方法基于加压液体萃取（PLE），然后通过固相萃取（SPE）进行净化和预浓缩，最后通过液相色谱-三重四极杆质谱仪（LC-QqQMS）进行定量。该方法根据分散剂类型、温度和萃取溶剂进行了优化。此外，还详细研究了沉积物中有机物对定量分析的影响。基质效应与保留时间高度显著相关（r=-0.9146，p < 0.0001）。在不影响方法灵敏度的情况下，使用内标物对基质效应进行有效校正的效果最佳。该方法的主要优点包括：线性（R2 > 0.990）、萃取回收率（34 种化合物的回收率 > 60%）、准确度（偏差 < 15%）、精密度（相对标准偏差 < 20%）和基质效应（-13.3% 至 17.8%）。该方法可用于不同沉积物基质中 TrOCs 的常规分析。该方法适用于在加拿大魁北克采集的 10 个湖泊沉积物样本。结果表明，至少有一个湖泊中存在 17 种化合物，浓度介于 0.07 至 1531 纳克 g-1 之间。所报告的浓度初步反映了加拿大东部高度人类化的小湖生态系统沉积物中化学胁迫物的存在情况。

{"title":"Method development and comprehensive study of matrix effects for the determination of trace organic contaminants in lake sediments","authors":"François-Xavier Teysseire , Hubert Cabana , Pedro A. Segura","doi":"10.1016/j.chroma.2024.465504","DOIUrl":"10.1016/j.chroma.2024.465504","url":null,"abstract":"<div><div>The presence of trace organic contaminants (TrOCs), such as pharmaceuticals, personal care products, additives, and polar pesticides in sediments of rivers and lakes highly impacted by anthropogenic activities makes sediments a secondary source of contamination for aquatic ecosystems. Considering this, a method for analyzing 44 TrOCs of diverse nature (including five transformation products, 13 pharmaceuticals, five personal care products, 14 pesticides, and seven additives) was developed and validated. It is based on extraction by pressurized liquid extraction (PLE), followed by purification and pre-concentration by solid phase extraction (SPE) and quantification by liquid chromatography coupled to a triple quadrupole mass spectrometer (LC-QqQMS). The method was optimized according to dispersant type, temperature, and extraction solvent. The influence of organic matter in sediments on quantitative analysis was also investigated in detail. Matrix effects were highly and significantly correlated (<em>r</em>=-0.9146, <em>p</em> < 0.0001) with retention time. Using internal standards showed the best results for effectively correcting matrix effects without affecting method sensitivity. The method was then validated according to key figures of merit: linearity (<em>R<sup>2</sup></em> > 0.990), extraction recoveries (> 60 % for 34 compounds), trueness (bias % < 15 %), precision (relative standard deviation < 20 %) and matrix effects (between -13.3 % and 17.8 %). This method can be applied for routine analysis of TrOCs in different sediment matrices. The method was applied to ten lake sediment samples collected in Québec, Canada. Results demonstrated the presence of 17 compounds in at least one lake at concentrations between 0.07 to 1531 ng g<sup>-1</sup>. The reported concentrations provide a first picture of the occurrence of chemical stressors in sediments of small lake highly anthropized ecosystems in Eastern Canada.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465504"},"PeriodicalIF":3.8,"publicationDate":"2024-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611227","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Metal organic framework derived composite as a new sorbent for micro-solid phase extraction of parabens from breast milk samples 将金属有机框架衍生复合材料作为一种新型吸附剂，用于从母乳样品中进行对羟基苯甲酸酯的微固相萃取。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-06 DOI: 10.1016/j.chroma.2024.465505

Hanieh Haghgouei , Shahram Seidi , Mahsa Shirkhodaie

In an attempt to enhance the adsorptive properties while addressing the limitations associated with powdered nature, zeolitic imidazolate framework (ZIF-67)-derived cobalt-doped nanoporous carbon (Co-NPC) was incorporated into chitosan and then shaped like hollow fiber by a simple casting method. Further modification with polyaniline (PANI) was also performed to improve extraction efficacy. The applicability of the modified hollow fibers was then investigated by packing them into a cartridge and utilizing them for conducting hollow fibers-packed in-cartridge micro solid-phase extraction (HF-IC µ-SPE) of parabens including methylparaben (MP), ethylparaben (EP), and propylparaben (PP) from human breast milk samples. Factors affecting extraction performance were studied using central composite design (CCD). Under the optimal conditions, good linearity was achieved within the range of 0.5–500 μg L⁻¹ with the determination coefficient (R²) higher than 0.9901. All analytical parameters were obtained by liquid chromatography-tandem mass spectrometry (LC–MS/MS) analysis. In this regard, the limits of detection values (LODs) were 0.5 to 1.0 μg L⁻¹. Intra- and inter-assay precision RSDs % were lower than 7.9 % and 8.4 %, respectively. Relative recoveries of breast milk samples were found in the range of 88.0–109.5 %. Accordingly, the novel nanocomposite sorbent based on PANI@Co-NPC/Chitosan hollow fiber was found to be an efficient, simple, and cost-effective packing material for HF-IC µ-SPE. It can also be offered as a promising alternative adsorbent to coated conventional hollow fiber.

为了提高吸附性能，同时解决与粉末性质相关的局限性，沸石咪唑酸框架（ZIF-67）衍生的掺钴纳米多孔碳（Co-NPC）被加入壳聚糖中，然后通过简单的铸造方法制成中空纤维。此外，还用聚苯胺（PANI）进行了进一步改性，以提高萃取效果。研究人员将改性后的中空纤维装入滤芯，并利用它们对母乳样品中的对羟基苯甲酸甲酯（MP）、对羟基苯甲酸乙酯（EP）和对羟基苯甲酸丙酯（PP）进行中空纤维装入滤芯的微固相萃取（HF-IC µ-SPE），从而考察了改性中空纤维的适用性。采用中心复合设计（CCD）对影响萃取性能的因素进行了研究。在最佳条件下，该方法在 0.5-500 μg L-1 范围内线性关系良好，测定系数 (R2) 大于 0.9901。所有分析参数均通过液相色谱-串联质谱（LC-MS/MS）分析获得。检测限为 0.5 至 1.0 μg L-1。测定内和测定间精密度 RSD 分别低于 7.9 % 和 8.4 %。母乳样品的相对回收率为 88.0-109.5%。因此，基于 PANI@Co-NPC/Chitosan 中空纤维的新型纳米复合吸附剂是一种高效、简单、经济的高频集成 µ-SPE 填料。它还可以作为涂覆传统中空纤维的一种有前途的替代吸附剂。

{"title":"Metal organic framework derived composite as a new sorbent for micro-solid phase extraction of parabens from breast milk samples","authors":"Hanieh Haghgouei , Shahram Seidi , Mahsa Shirkhodaie","doi":"10.1016/j.chroma.2024.465505","DOIUrl":"10.1016/j.chroma.2024.465505","url":null,"abstract":"<div><div>In an attempt to enhance the adsorptive properties while addressing the limitations associated with powdered nature, zeolitic imidazolate framework (ZIF-67)-derived cobalt-doped nanoporous carbon (Co-NPC) was incorporated into chitosan and then shaped like hollow fiber by a simple casting method. Further modification with polyaniline (PANI) was also performed to improve extraction efficacy. The applicability of the modified hollow fibers was then investigated by packing them into a cartridge and utilizing them for conducting hollow fibers-packed in-cartridge micro solid-phase extraction (HF-IC µ-SPE) of parabens including methylparaben (MP), ethylparaben (EP), and propylparaben (PP) from human breast milk samples. Factors affecting extraction performance were studied using central composite design (CCD). Under the optimal conditions, good linearity was achieved within the range of 0.5–500 μg L<sup>−1</sup> with the determination coefficient (<em>R</em><sup>2</sup>) higher than 0.9901. All analytical parameters were obtained by liquid chromatography-tandem mass spectrometry (LC–MS/MS) analysis. In this regard, the limits of detection values (LODs) were 0.5 to 1.0 μg L<sup>−1</sup>. Intra- and inter-assay precision RSDs % were lower than 7.9 % and 8.4 %, respectively. Relative recoveries of breast milk samples were found in the range of 88.0–109.5 %. Accordingly, the novel nanocomposite sorbent based on PANI@Co-NPC/Chitosan hollow fiber was found to be an efficient, simple, and cost-effective packing material for HF-IC µ-SPE. It can also be offered as a promising alternative adsorbent to coated conventional hollow fiber.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465505"},"PeriodicalIF":3.8,"publicationDate":"2024-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611225","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Harnessing the resolution power of two-dimensional liquid chromatography (2D-LC) for the screening of bisphenol contaminants in canned food items 利用二维液相色谱（2D-LC）的分辨能力筛查罐头食品中的双酚污染物。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-04 DOI: 10.1016/j.chroma.2024.465502

Sumayyah A.B. Chotoye, N. Patricia Granados, Christa L. Brosseau

Overlapping peaks can be difficult to avoid in 1D-LC, which make the identification and quantification of compounds ambiguous, especially if the only available detector is a UV/DAD. To overcome this, a two-dimensional liquid chromatography (2D-LC) method to monitor Bisphenols (BPs), and particularly the chosen analogues BPA, BPB, BPF, BPS, BPZ, and BPAF, in a complex matrix (canned food) was developed and validated. BPs are endocrine disruptors present in the lining of the can, which may leach into the content of canned food. It is essential to continuously identify and monitor bisphenols that are unintentionally ingested using newly available and highly efficient methods such as 2D-LC. The coefficient of variation (CV) of peak areas and retention times for all analytes in both dimensions ranged from 0.050 to 2.960 %. The recovery of the whole procedure was determined to be 67.4 ± 0.1 % in the first dimension, and 64.3 ± 0.1 % in the second dimension. The limit of detection (LOD) determined in the second dimension for the analytes ranged from 0.075 to 0.301 ppm. Finally, four canned food samples were prepared by solid-liquid extraction, and surveyed for BPA, BPB, BPF, BPS, BPZ, and BPAF. BPF (0.093 ppm) and BPAF (2.656 ppm) were accurately detected in two separate samples. This report highlights the first successful application of 2D-LC to bisphenol compounds, an important class of emerging contaminants.

在一维液相色谱法中很难避免重叠峰的出现，这使得化合物的鉴定和定量变得模糊不清，尤其是在唯一可用的检测器是 UV/DAD 的情况下。为了克服这一问题，我们开发并验证了一种二维液相色谱（2D-LC）方法，用于监测复杂基质（罐装食品）中的双酚（BPs），特别是所选类似物双酚 A、双酚 B、双酚 F、双酚 S、双酚 Z 和双酚 F。双酚 A 是存在于罐头内衬中的内分泌干扰物，可能会渗入罐头食品的内容物中。使用新推出的高效方法（如 2D-LC 方法）持续识别和监测无意摄入的双酚是非常重要的。所有分析物在两个维度上的峰面积和保留时间的变异系数 (CV) 在 0.050% 到 2.960% 之间。整个过程的回收率在一维为 67.4 ± 0.1 %，在二维为 64.3 ± 0.1 %。在第二维度中确定的分析物检测限（LOD）为 0.075 至 0.301 ppm。最后，采用固液萃取法制备了四种罐头食品样品，并对其中的双酚 A、双酚 B、双酚 F、双酚 S、双酚 Z 和双酚 AF 进行了检测。在两个不同的样品中准确地检测到了 BPF（0.093 ppm）和 BPAF（2.656 ppm）。本报告强调了 2D-LC 在双酚化合物（一类重要的新兴污染物）中的首次成功应用。

{"title":"Harnessing the resolution power of two-dimensional liquid chromatography (2D-LC) for the screening of bisphenol contaminants in canned food items","authors":"Sumayyah A.B. Chotoye, N. Patricia Granados, Christa L. Brosseau","doi":"10.1016/j.chroma.2024.465502","DOIUrl":"10.1016/j.chroma.2024.465502","url":null,"abstract":"<div><div>Overlapping peaks can be difficult to avoid in 1D-LC, which make the identification and quantification of compounds ambiguous, especially if the only available detector is a UV/DAD. To overcome this, a two-dimensional liquid chromatography (2D-LC) method to monitor Bisphenols (BPs), and particularly the chosen analogues BPA, BPB, BPF, BPS, BPZ, and BPAF, in a complex matrix (canned food) was developed and validated. BPs are endocrine disruptors present in the lining of the can, which may leach into the content of canned food. It is essential to continuously identify and monitor bisphenols that are unintentionally ingested using newly available and highly efficient methods such as 2D-LC. The coefficient of variation (CV) of peak areas and retention times for all analytes in both dimensions ranged from 0.050 to 2.960 %. The recovery of the whole procedure was determined to be 67.4 ± 0.1 % in the first dimension, and 64.3 ± 0.1 % in the second dimension. The limit of detection (LOD) determined in the second dimension for the analytes ranged from 0.075 to 0.301 ppm. Finally, four canned food samples were prepared by solid-liquid extraction, and surveyed for BPA, BPB, BPF, BPS, BPZ, and BPAF. BPF (0.093 ppm) and BPAF (2.656 ppm) were accurately detected in two separate samples. This report highlights the first successful application of 2D-LC to bisphenol compounds, an important class of emerging contaminants.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465502"},"PeriodicalIF":3.8,"publicationDate":"2024-11-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611212","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Evaluation of size-based distribution of components in VYXEOS® liposomal formulation using asymmetric flow field-flow fractionation 利用非对称流场-流动分馏法评估 VYXEOS® 脂质体配方中基于粒度的成分分布。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-03 DOI: 10.1016/j.chroma.2024.465488

Dumindika A. Siriwardane , Sheyda Shakiba , Wenlei Jiang , Thilak Mudalige

VYXEOS® is the first FDA-approved dual-API liposomal formulation containing two different chemotherapeutics, daunorubicin and cytarabine at a 1:5 molar ratio. Analysis of bulk formulation does not provide insight to size-based distribution of APIs and excipients, therefore asymmetrical flow field-flow fractionation (AF4) was utilized for the size-based separation of VYXEOS® liposomes and collected size fractions were further analyzed for the concentrations of APIs, lipid excipients, and copper. Analysis results revealed a significant variation in API distribution across the size fractions, with the larger liposomes encapsulating a higher ratio of cytarabine to daunorubicin compared to the smaller liposomes, while lipid excipient composition was held constant across the size range. We attribute the size-based variation of API ratios to structural change during API loading and sequence of API loading. Cytarabine is first passively loaded into liposomes containing copper gluconate, and then daunorubicin is actively loaded using copper gradient where the daunorubicin is retained in the liposomes as a copper complex. This method can be extended to characterize various single and dual-API liposomal nanocarriers during drug product development and/or post market quality control.

VYXEOS® 是首个获得 FDA 批准的双 API 脂质体制剂，含有两种不同的化疗药物，即 1:5 摩尔比的达乌比星和阿糖胞苷。对散装制剂的分析无法深入了解原料药和辅料的粒度分布，因此采用了非对称流场-流动分馏（AF4）技术对 VYXEOS® 脂质体进行粒度分离，并对收集的粒度分馏物进一步分析原料药、脂质辅料和铜的浓度。分析结果表明，不同粒度的脂质体中原料药的分布存在明显差异，与较小的脂质体相比，较大的脂质体中包裹的阿糖胞苷和达乌诺比星的比例更高，而不同粒度的脂质辅料成分保持不变。我们将原料药比例的大小变化归因于原料药装载过程中的结构变化和原料药装载顺序。首先将阿糖胞苷被动地装入含有葡萄糖酸铜的脂质体，然后使用铜梯度主动装入达柔比星，在此过程中，达柔比星作为铜复合物保留在脂质体中。该方法可在药物产品开发和/或上市后质量控制过程中，扩展用于表征各种单API和双API脂质体纳米载体。

{"title":"Evaluation of size-based distribution of components in VYXEOS® liposomal formulation using asymmetric flow field-flow fractionation","authors":"Dumindika A. Siriwardane , Sheyda Shakiba , Wenlei Jiang , Thilak Mudalige","doi":"10.1016/j.chroma.2024.465488","DOIUrl":"10.1016/j.chroma.2024.465488","url":null,"abstract":"<div><div>VYXEOS® is the first FDA-approved dual-API liposomal formulation containing two different chemotherapeutics, daunorubicin and cytarabine at a 1:5 molar ratio. Analysis of bulk formulation does not provide insight to size-based distribution of APIs and excipients, therefore asymmetrical flow field-flow fractionation (AF4) was utilized for the size-based separation of VYXEOS® liposomes and collected size fractions were further analyzed for the concentrations of APIs, lipid excipients, and copper. Analysis results revealed a significant variation in API distribution across the size fractions, with the larger liposomes encapsulating a higher ratio of cytarabine to daunorubicin compared to the smaller liposomes, while lipid excipient composition was held constant across the size range. We attribute the size-based variation of API ratios to structural change during API loading and sequence of API loading. Cytarabine is first passively loaded into liposomes containing copper gluconate, and then daunorubicin is actively loaded using copper gradient where the daunorubicin is retained in the liposomes as a copper complex. This method can be extended to characterize various single and dual-API liposomal nanocarriers during drug product development and/or post market quality control.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465488"},"PeriodicalIF":3.8,"publicationDate":"2024-11-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142602208","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Cost-effective synthesis and application of Cu²⁺-doped melamine formaldehyde resin for enhanced tetracycline enrichment in environmental water 掺杂 Cu²⁺ 的三聚氰胺甲醛树脂的成本效益合成与应用，用于提高环境水体中四环素的富集度。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-02 DOI: 10.1016/j.chroma.2024.465499

Lin Gu , Junyu Zhang , Shuhai Ding , Longlong Wang , Wei Xia , Peng Wang , Wenlei Zhai , Cong Kong , Xiaosheng Shen , Chengqi Fan , Guangxin Yang

Tetracycline antibiotics (TCs) are typically present at low residue levels in environmental water, necessitating enrichment prior to analysis. In this study, a Cu²⁺-doped melamine formaldehyde resin (Cu-MFR) was synthesized to enhance the adsorption efficiency for TCs, leveraging the formation of stable Cu²⁺-TC complexes on the sorbent surface. Then it was used as an adsorbent in solid-phase extraction (SPE) for the enrichment of four TCs from water samples. The optimized parameters for Cu-MFR in the analysis of TCs in environmental water enabled linear detection ranges from 0.20 to 50 ng/mL, with relative recoveries ranging from 79.5 % to 97.6 % and relative standard deviations ≤ 10.0 %, using high-performance liquid chromatography-tandem high-resolution mass spectrometry (HPLC-HRMS). The limits of detection for the four TCs were determined to be between 0.11 and 0.16 ng/mL, indicating its potential for practical application in real sample analysis.

四环素类抗生素（TC）在环境水体中的残留量通常很低，因此需要在分析前进行富集。本研究合成了一种掺杂 Cu2+ 的三聚氰胺甲醛树脂（Cu-MFR），通过在吸附剂表面形成稳定的 Cu2+-TC 复合物来提高 TCs 的吸附效率。然后将其作为固相萃取（SPE）中的吸附剂，用于富集水样中的四种三氯甲烷。利用高效液相色谱-串联高分辨质谱法（HPLC-HRMS）分析环境水样中的 TCs，Cu-MFR 的优化参数可实现 0.20 至 50 ng/mL 的线性检测范围，相对回收率为 79.5 % 至 97.6 %，相对标准偏差小于 10.0 %。四种三氯乙酸的检测限被确定为 0.11 至 0.16 纳克/毫升，这表明该方法在实际样品分析中具有实际应用潜力。

{"title":"Cost-effective synthesis and application of Cu²⁺-doped melamine formaldehyde resin for enhanced tetracycline enrichment in environmental water","authors":"Lin Gu , Junyu Zhang , Shuhai Ding , Longlong Wang , Wei Xia , Peng Wang , Wenlei Zhai , Cong Kong , Xiaosheng Shen , Chengqi Fan , Guangxin Yang","doi":"10.1016/j.chroma.2024.465499","DOIUrl":"10.1016/j.chroma.2024.465499","url":null,"abstract":"<div><div>Tetracycline antibiotics (TCs) are typically present at low residue levels in environmental water, necessitating enrichment prior to analysis. In this study, a Cu<sup>2+</sup>-doped melamine formaldehyde resin (Cu-MFR) was synthesized to enhance the adsorption efficiency for TCs, leveraging the formation of stable Cu<sup>2+</sup>-TC complexes on the sorbent surface. Then it was used as an adsorbent in solid-phase extraction (SPE) for the enrichment of four TCs from water samples. The optimized parameters for Cu-MFR in the analysis of TCs in environmental water enabled linear detection ranges from 0.20 to 50 ng/mL, with relative recoveries ranging from 79.5 % to 97.6 % and relative standard deviations ≤ 10.0 %, using high-performance liquid chromatography-tandem high-resolution mass spectrometry (HPLC-HRMS). The limits of detection for the four TCs were determined to be between 0.11 and 0.16 ng/mL, indicating its potential for practical application in real sample analysis.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465499"},"PeriodicalIF":3.8,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142611208","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

An efficient PCN-224/graphene aerogel-based extraction method for monitoring the degradation of organophosphorus pesticides in juice 基于 PCN-224/ 石墨烯气凝胶的高效萃取法监测果汁中有机磷农药的降解情况

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-02 DOI: 10.1016/j.chroma.2024.465500

Zirou Wang , Sitian Gu , Yu Ma , Huixiao Duo , Wei Wu , Qingli Yang , Xiudan Hou

An efficient PCN-224/graphene aerogel modified silica (PCN-224/GA@Sil)-based extraction method was established for monitoring the degradation process of two organophosphorus pesticides (OPPs) in juice. PCN-224/GA@Sil exhibited higher surface area (307.35 m² g^-1) than graphene oxide modified silica (254.09 m² g^-1). The introduction of PCN-224 endowed the sorbent with excellent adsorption specificity towards OPPs due to the ZrˑˑˑS/O coordination bond. PCN-224 exhibited relatively higher theoretical adsorption energies of PCN-224 towards fenitrothion and fenthion were 0.68 eV and -0.31 eV. The established PCN-224/GA@Sil-HPLC method showed the linearity of 0.2–500 μg L^-1 for analytes. The matrix effects in juice were 9.68 % and 3.61 % for fenitrothion and fenthion. Finally, it was used for the sample pretreatment of juice preventing interference from food matrices to monitor the degradation of two OPPs. A combination method of ultrasound and xenon lamp was adopted to degrade fenitrothion and fenthion displaying the synergistic effect (SE=2.12, 1.39).

建立了一种基于PCN-224/石墨烯气凝胶修饰二氧化硅（PCN-224/GA@Sil）的高效萃取方法，用于监测果汁中两种有机磷农药（OPPs）的降解过程。PCN-224/GA@Sil 的比表面积（307.35 m2 g-1）高于氧化石墨烯修饰的二氧化硅（254.09 m2 g-1）。由于 ZrˑˑˑS/O 配位键的作用，PCN-224 的引入使吸附剂对 OPPs 具有极佳的吸附特异性。PCN-224 对杀螟硫磷和倍硫磷的理论吸附能相对较高，分别为 0.68 eV 和 -0.31 eV。PCN-224/GA@Sil-HPLC方法的线性范围为0.2～500 μg L-1。果汁中杀螟硫磷和倍硫磷的基质效应分别为 9.68 % 和 3.61 %。最后，该方法被用于果汁样品的预处理，以防止食物基质的干扰，从而监测两种 OPPs 的降解情况。采用超声波和氙灯组合方法降解杀螟松和倍硫磷显示出协同效应（SE=2.12，1.39）。

{"title":"An efficient PCN-224/graphene aerogel-based extraction method for monitoring the degradation of organophosphorus pesticides in juice","authors":"Zirou Wang , Sitian Gu , Yu Ma , Huixiao Duo , Wei Wu , Qingli Yang , Xiudan Hou","doi":"10.1016/j.chroma.2024.465500","DOIUrl":"10.1016/j.chroma.2024.465500","url":null,"abstract":"<div><div>An efficient PCN-224/graphene aerogel modified silica (PCN-224/GA@Sil)-based extraction method was established for monitoring the degradation process of two organophosphorus pesticides (OPPs) in juice. PCN-224/GA@Sil exhibited higher surface area (307.35 m<sup>2</sup> g<sup>-1</sup>) than graphene oxide modified silica (254.09 m<sup>2</sup> g<sup>-1</sup>). The introduction of PCN-224 endowed the sorbent with excellent adsorption specificity towards OPPs due to the ZrˑˑˑS/O coordination bond. PCN-224 exhibited relatively higher theoretical adsorption energies of PCN-224 towards fenitrothion and fenthion were 0.68 eV and -0.31 eV. The established PCN-224/GA@Sil-HPLC method showed the linearity of 0.2–500 μg L<sup>-1</sup> for analytes. The matrix effects in juice were 9.68 % and 3.61 % for fenitrothion and fenthion. Finally, it was used for the sample pretreatment of juice preventing interference from food matrices to monitor the degradation of two OPPs. A combination method of ultrasound and xenon lamp was adopted to degrade fenitrothion and fenthion displaying the synergistic effect (<em>SE</em>=2.12, 1.39).</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465500"},"PeriodicalIF":3.8,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142592739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Unlocking the future of colorectal cancer detection: Advances in screening glycosylation-based biomarkers on biological mass spectrometry technology 开启结直肠癌检测的未来：利用生物质谱技术筛选糖基化生物标记物的进展

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-02 DOI: 10.1016/j.chroma.2024.465501

Yuxuan Li , Songze Wang , Chengqiang Han , Xi-Ling Li, Jun Zhe Min

The incidence of colorectal cancer (CRC) is increasingly affecting younger populations, with its mortality rate rising annually. However, current clinical diagnostic techniques, such as colonoscopy and CEA antigen testing, remain invasive and prone to false-positive results, complicating early diagnosis and intervention. Glycosylation, a key post-translational modification, plays an essential role in cellular function, physiological regulation, and disease processes. In recent years, mass spectrometry technology has emerged as a powerful tool for screening glycan biomarkers, owing to its exceptional separation capabilities and sensitivity. This review encompasses the advancements in CRC glycan biomarkers from 2016 to 2024, with particular emphasis placed on N/O-glycan biomarkers identified through mass spectrometry. Nonetheless, the intrinsic low abundance and polyhydroxy nature of glycans hinder the specificity and sensitivity of current glycan biomarkers. To overcome these limitations, this article outlines pretreatment strategies for N/O-glycans, including glycan release, enrichment, purification, and derivatization, in conjunction with relative quantification techniques and high-throughput bioinformatics tools for biomarker screening. These strategies are anticipated to enhance the efficiency and precision of glycan biomarker identification through mass spectrometry. These advancements hold significant promise for enhancing CRC prevention, diagnosis, and treatment, thereby potentially improving patient outcomes and quality of life.

结肠直肠癌（CRC）的发病率正日益影响年轻人群，其死亡率也在逐年上升。然而，目前的临床诊断技术，如结肠镜检查和癌胚抗原检测，仍然具有侵入性，而且容易出现假阳性结果，使早期诊断和干预变得复杂。糖基化是一种关键的翻译后修饰，在细胞功能、生理调节和疾病过程中起着至关重要的作用。近年来，质谱技术凭借其卓越的分离能力和灵敏度成为筛选糖类生物标记物的有力工具。本综述涵盖了 2016 年至 2024 年期间 CRC 糖类生物标志物的研究进展，其中特别强调了通过质谱技术鉴定的 N/O 糖类生物标志物。然而，聚糖固有的低丰度和多羟基性质阻碍了目前聚糖生物标志物的特异性和灵敏度。为了克服这些局限性，本文概述了 N/O 聚糖的预处理策略，包括聚糖释放、富集、纯化和衍生化，并结合相对定量技术和高通量生物信息学工具进行生物标记物筛选。预计这些策略将提高通过质谱鉴定聚糖生物标记物的效率和精确度。这些进展为加强 CRC 的预防、诊断和治疗带来了巨大希望，从而有可能改善患者的预后和生活质量。

{"title":"Unlocking the future of colorectal cancer detection: Advances in screening glycosylation-based biomarkers on biological mass spectrometry technology","authors":"Yuxuan Li , Songze Wang , Chengqiang Han , Xi-Ling Li, Jun Zhe Min","doi":"10.1016/j.chroma.2024.465501","DOIUrl":"10.1016/j.chroma.2024.465501","url":null,"abstract":"<div><div>The incidence of colorectal cancer (CRC) is increasingly affecting younger populations, with its mortality rate rising annually. However, current clinical diagnostic techniques, such as colonoscopy and CEA antigen testing, remain invasive and prone to false-positive results, complicating early diagnosis and intervention. Glycosylation, a key post-translational modification, plays an essential role in cellular function, physiological regulation, and disease processes. In recent years, mass spectrometry technology has emerged as a powerful tool for screening glycan biomarkers, owing to its exceptional separation capabilities and sensitivity. This review encompasses the advancements in CRC glycan biomarkers from 2016 to 2024, with particular emphasis placed on N/O-glycan biomarkers identified through mass spectrometry. Nonetheless, the intrinsic low abundance and polyhydroxy nature of glycans hinder the specificity and sensitivity of current glycan biomarkers. To overcome these limitations, this article outlines pretreatment strategies for N/O-glycans, including glycan release, enrichment, purification, and derivatization, in conjunction with relative quantification techniques and high-throughput bioinformatics tools for biomarker screening. These strategies are anticipated to enhance the efficiency and precision of glycan biomarker identification through mass spectrometry. These advancements hold significant promise for enhancing CRC prevention, diagnosis, and treatment, thereby potentially improving patient outcomes and quality of life.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465501"},"PeriodicalIF":3.8,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142586869","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Enhancing coverage of annotated compounds in traditional Chinese medicine formulas: Integrating MSE and Fast-DDA molecular network with AntDAS—Case study of Xiao Jian Zhong Tang 提高中药配方中已注释化合物的覆盖率：将 MSE 和 Fast-DDA 分子网络与 AntDAS 相结合--小建中汤案例研究

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-11-01 DOI: 10.1016/j.chroma.2024.465498

Xiaojing Cui , Pingping Liu , Xingyue Huang , Yongjie Yu , Xuemei Qin , Huina Zhou , Qingxia Zheng , Yuetao Liu

The chemical characterisation of traditional Chinese medicine formulas (TCMFs) using mass spectrometry poses notable challenges owing to their complex and diverse chemical compositions. While acquisition modes such as data-dependent acquisition (DDA) and data-independent acquisition (DIA) offer new insights, DDA's tendency to overlook low-abundance ions and DIA's complicated data processing, particularly in matching MS¹ and MS² information, limit the effective annotation of valuable compounds in TCMFs. Herein, we present a new integrated strategy to enhance the coverage of annotated compounds in TCMFs, using Xiao Jian Zhong Tang (XJZ) as a case study. First, we characterised the components of XJZ through UNIFI software in Fast-DDA and DIA modes. We then summarised the diagnostic ions and substituent information of the identified compounds based on the Fast-DDA data, integrating molecular networks and AntDAS to predict unknown components and uncover potential components. Ultimately, we characterised a total of 785 components in XJZ, including 43 that were unique to XJZ when compared to the individual herbs involved. The presence of these new components may result from the recombination of substituents during compatibility. In conclusion, this new integrated strategy facilitates more in-depth characterisation of components in TCMFs, providing a new direction for exploring the compatibility principles among TCMFs.

由于传统中药配方（TCMFs）的化学成分复杂多样，使用质谱对其进行化学特征描述具有显著的挑战性。虽然数据依赖采集（DDA）和数据独立采集（DIA）等采集模式能提供新的见解，但DDA容易忽略低丰度离子，DIA数据处理复杂，特别是在匹配MS1和MS2信息时，限制了对中药方剂中有价值化合物的有效注释。在此，我们以小建中堂（XJZ）为例，提出了一种新的综合策略，以提高中药论坛中已注释化合物的覆盖率。首先，我们通过 UNIFI 软件在快速-DDA 和 DIA 模式下表征了 XJZ 的成分。然后，我们根据快速 DDA 数据总结了已鉴定化合物的诊断离子和取代基信息，并结合分子网络和 AntDAS 预测未知成分和发现潜在成分。最终，我们共鉴定出 XJZ 中的 785 种成分，其中包括 43 种 XJZ 独有的成分。这些新成分的出现可能是在兼容过程中取代基重组的结果。总之，这一新的综合策略有助于对中药成分进行更深入的表征，为探索中药成分间的相容性原理提供了新的方向。

{"title":"Enhancing coverage of annotated compounds in traditional Chinese medicine formulas: Integrating MSE and Fast-DDA molecular network with AntDAS—Case study of Xiao Jian Zhong Tang","authors":"Xiaojing Cui , Pingping Liu , Xingyue Huang , Yongjie Yu , Xuemei Qin , Huina Zhou , Qingxia Zheng , Yuetao Liu","doi":"10.1016/j.chroma.2024.465498","DOIUrl":"10.1016/j.chroma.2024.465498","url":null,"abstract":"<div><div>The chemical characterisation of traditional Chinese medicine formulas (TCMFs) using mass spectrometry poses notable challenges owing to their complex and diverse chemical compositions. While acquisition modes such as data-dependent acquisition (DDA) and data-independent acquisition (DIA) offer new insights, DDA's tendency to overlook low-abundance ions and DIA's complicated data processing, particularly in matching MS<sup>1</sup> and MS<sup>2</sup> information, limit the effective annotation of valuable compounds in TCMFs. Herein, we present a new integrated strategy to enhance the coverage of annotated compounds in TCMFs, using Xiao Jian Zhong Tang (XJZ) as a case study. First, we characterised the components of XJZ through UNIFI software in Fast-DDA and DIA modes. We then summarised the diagnostic ions and substituent information of the identified compounds based on the Fast-DDA data, integrating molecular networks and AntDAS to predict unknown components and uncover potential components. Ultimately, we characterised a total of 785 components in XJZ, including 43 that were unique to XJZ when compared to the individual herbs involved. The presence of these new components may result from the recombination of substituents during compatibility. In conclusion, this new integrated strategy facilitates more in-depth characterisation of components in TCMFs, providing a new direction for exploring the compatibility principles among TCMFs.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465498"},"PeriodicalIF":3.8,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142586868","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Rapid on-site detection of illicit drugs in urine using C18 pipette-tip based solid-phase extraction coupled with a miniaturized mass spectrometer 使用基于 C18 移液管吸头的固相萃取技术和微型质谱仪现场快速检测尿液中的违禁药物。

IF 3.8 2区化学 Q1 BIOCHEMICAL RESEARCH METHODS

Journal of Chromatography A

Pub Date : 2024-10-30 DOI: 10.1016/j.chroma.2024.465485

Jiahui Wu , Yunfeng Zhang , Manman Zhang , Linpei Dong , Bo Zou , Jiabin Jin , Yong Liu , Danxia Yu , Yu Xu , Yilei Fan , Zheng Ouyang , Qing Shen , Haixing Wang

Drug abuse is a social issue worldwide, and there is an increasing demand for on-site rapid detection of illicit drugs. In this study, a rapid and simple analytical method for the detection of 6-monoacetylmorphine (6-MAM), methamphetamine (MA), methylenedioxymethamphetamine (MDMA), ketamine (K), norketamine (NK), and cocaine (COC) in urine was developed. The developed method combines C18 pipette-tip based solid-phase extraction (C18 PT-SPE) with a miniaturized mass spectrometer (miniMS), exhibiting remarkable simplicity, high sensitivity, and strong reliability, compared with the conventional method. The optimal extraction and elution conditions for C18 PT-SPE were considered as 9 and 3 aspirating-dispensing cycles, respectively. The miniMS parameters including spray voltage, isolation potential, and collision-induced dissociation energy for the detection of these six illicit drugs were optimized using a nano-electrospray ionization method. The limit of detection (LOD), limit of quantification (LOQ), linear range, and linearity for the analysis of six illicit drugs in urine with the proposed C18 PT-SPE-miniMS method were determined. Except for the LOD of K and COC was determined as 0.5 and 0.25 ng mL⁻¹ respectively, and the LOD of 6-MAM MA, MDMA, and NK was determined as 1 ng mL⁻¹. This method enables rapid on-site detection, providing easier operation, lower cost, and better portability compared to conventional methods, making it a potential tool in drug crime investigation and forensic science.

药物滥用是一个全球性的社会问题，对现场快速检测非法药物的需求日益增加。本研究建立了一种快速、简便的分析方法，用于检测尿液中的 6-单乙酰吗啡（6-MAM）、甲基苯丙胺（MA）、亚甲二氧基甲基苯丙胺（MDMA）、氯胺酮（K）、诺基他明（NK）和可卡因（COC）。该方法将C18吸头固相萃取（C18 PT-SPE）与微型质谱仪（miniMS）相结合，与传统方法相比，具有简便、灵敏度高、可靠性强等特点。C18 PT-SPE的最佳萃取和洗脱条件分别为9次和3次吸气-分配循环。采用纳米电喷雾离子化方法优化了检测这六种违禁药物的miniMS参数，包括喷雾电压、分离电位和碰撞诱导解离能。确定了采用所提议的 C18 PT-SPE-miniMS 方法分析尿液中六种违禁药物的检出限（LOD）、定量限（LOQ）、线性范围和线性度。除 K 和 COC 的检出限分别为 0.5 和 0.25 ng mL-1 外，6-MAM MA、MDMA 和 NK 的检出限均为 1 ng mL-1。与传统方法相比，该方法操作简便、成本低廉、便于携带，可实现现场快速检测，是毒品犯罪调查和法医学研究的一种潜在工具。

{"title":"Rapid on-site detection of illicit drugs in urine using C18 pipette-tip based solid-phase extraction coupled with a miniaturized mass spectrometer","authors":"Jiahui Wu , Yunfeng Zhang , Manman Zhang , Linpei Dong , Bo Zou , Jiabin Jin , Yong Liu , Danxia Yu , Yu Xu , Yilei Fan , Zheng Ouyang , Qing Shen , Haixing Wang","doi":"10.1016/j.chroma.2024.465485","DOIUrl":"10.1016/j.chroma.2024.465485","url":null,"abstract":"<div><div>Drug abuse is a social issue worldwide, and there is an increasing demand for on-site rapid detection of illicit drugs. In this study, a rapid and simple analytical method for the detection of 6-monoacetylmorphine (6-MAM), methamphetamine (MA), methylenedioxymethamphetamine (MDMA), ketamine (K), norketamine (NK), and cocaine (COC) in urine was developed. The developed method combines C18 pipette-tip based solid-phase extraction (C18 PT-SPE) with a miniaturized mass spectrometer (miniMS), exhibiting remarkable simplicity, high sensitivity, and strong reliability, compared with the conventional method. The optimal extraction and elution conditions for C18 PT-SPE were considered as 9 and 3 aspirating-dispensing cycles, respectively. The miniMS parameters including spray voltage, isolation potential, and collision-induced dissociation energy for the detection of these six illicit drugs were optimized using a nano-electrospray ionization method. The limit of detection (LOD), limit of quantification (LOQ), linear range, and linearity for the analysis of six illicit drugs in urine with the proposed C18 PT-SPE-miniMS method were determined. Except for the LOD of K and COC was determined as 0.5 and 0.25 ng mL<sup>−1</sup> respectively, and the LOD of 6-MAM MA, MDMA, and NK was determined as 1 ng mL<sup>−1</sup>. This method enables rapid on-site detection, providing easier operation, lower cost, and better portability compared to conventional methods, making it a potential tool in drug crime investigation and forensic science.</div></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":"1738 ","pages":"Article 465485"},"PeriodicalIF":3.8,"publicationDate":"2024-10-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142602246","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0