Journal of chromatography open最新文献_第7页

Multitargeted analysis for the simultaneous determination of organochlorine pesticides and polychlorinated biphenyls in sediments exploiting comprehensive two-dimensional gas chromatography coupled to mass spectrometry 综合二维气相色谱-质谱联用技术用于沉积物中有机氯农药和多氯联苯的多目标分析

IF 3.2

Journal of chromatography open

Pub Date : 2025-08-07 DOI: 10.1016/j.jcoa.2025.100245

Allan Polidoro , Valentina Costa , Monica Romagnoli , Elena Sarti , Claudia Stevanin , Cinzia Fabbro , Luisa Pasti , Flavio A. Franchina

Persistent organic pollutants (POPs), including organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs), remain a significant environmental concern due to their persistence, bioaccumulation, and toxicity. Accurate quantification of these contaminants in sediment matrices remains analytically challenging due to the complexity of the matrix and the need for detection at trace levels to meet regulatory standards. This research focused on the development and application of an analytical protocol for the simultaneous determination of OCPs and PCBs in sediments using solid-phase extraction (SPE) followed by comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry (GC×GC-TOFMS). The developed method was validated, achieving low limits of detection (0.4 to 14 ng kg^-1) and quantification (1.1 to 41 ng kg^-1), with satisfactory linearity (r² > 0.99), accuracy (90–110%), and precision (RSD < 5%) for all target analytes. Validation with certified reference material confirmed the agreement between experimental and certified concentrations for most compounds. The protocol was applied to environmental sediment samples, detecting multiple PCBs and DDT-related compounds at concentrations below international guideline values. These results confirm the method’s suitability for trace-level determination of OCPs and PCBs in sediments, addressing the analytical demands of environmental monitoring and regulatory compliance. The established protocol enables sensitive and reliable assessment of sediment contamination, supporting a simultaneous ongoing surveillance and risk assessment of such classes of persistent organic pollutants in the same analytical run.

持久性有机污染物（POPs），包括有机氯农药（ocp）和多氯联苯（PCBs），由于其持久性、生物蓄积性和毒性，仍然是一个重大的环境问题。由于基质的复杂性和需要在痕量水平检测以满足监管标准，对沉积物基质中这些污染物的准确定量分析仍然具有挑战性。本研究的重点是开发和应用一种同时测定沉积物中OCPs和pcb的分析方案，该分析方案采用固相萃取（SPE）和综合二维气相色谱-飞行时间质谱法（GC×GC-TOFMS）。验证了该方法的低检出限（0.4 ~ 14 ng kg-1）和定量限（1.1 ~ 41 ng kg-1），线性良好(r²>；0.99)，准确度（90-110%），精密度(RSD <；5%)用于所有目标分析物。经认证的标准物质验证证实了大多数化合物的实验浓度和认证浓度之间的一致性。该方案适用于环境沉积物样品，检测浓度低于国际指标值的多种多氯联苯和ddt相关化合物。这些结果证实了该方法适用于沉积物中痕量OCPs和多氯联苯的测定，满足了环境监测和法规遵从性的分析需求。已建立的协议能够对沉积物污染进行敏感和可靠的评估，支持在同一分析运行中同时对这类持久性有机污染物进行持续监测和风险评估。

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引用次数: 0

A tutorial on the synthesis and applications of molecularly imprinted polymers in analytical chemistry 分子印迹聚合物的合成及其在分析化学中的应用

IF 3.2

Journal of chromatography open

Pub Date : 2025-07-28 DOI: 10.1016/j.jcoa.2025.100244

N.P. Kalogiouri , A. Kabir , K.G. Furton , V.F. Samanidou

Molecularly imprinted polymers (MIPs) have emerged as highly selective sorbents with tailor-made recognition sites complementary to target analytes in terms of shape, size, and functional groups. This tutorial provides a comprehensive overview of the principles, synthesis strategies, and analytical applications of MIPs, with a focus on their utility in sample preparation, separation, and detection. Various imprinting techniques—such as bulk, surface, and nanoimprinting—are discussed alongside advances in green synthesis and novel monomer-template systems. Emphasis is placed on the integration of MIPs with chromatographic and spectrometric platforms, particularly in complex matrices relevant to environmental, pharmaceutical, food, and clinical analysis. The tutorial illustrates the practical considerations for designing and optimizing MIP-based methods, including template selection, polymerization conditions, and reusability, reflecting recent and relevant advances of the last ten years This tutorial aims to guide researchers and analysts in leveraging the unique properties of MIPs to enhance selectivity, sensitivity, and sustainability in modern analytical chemistry.

分子印迹聚合物（MIPs）已成为高度选择性的吸附剂，具有定制的识别位点，在形状、大小和官能团方面与目标分析物互补。本教程提供了原理的全面概述，合成策略，和MIPs的分析应用，重点是他们在样品制备，分离和检测的效用。各种印迹技术-如体、表面和纳米印迹-讨论了绿色合成和新型单体模板系统的进展。重点放在MIPs与色谱和光谱平台的集成上，特别是在与环境、制药、食品和临床分析相关的复杂基质中。本教程阐述了设计和优化基于mip的方法的实际考虑，包括模板选择，聚合条件和可重用性，反映了过去十年的最新和相关进展。本教程旨在指导研究人员和分析人员利用mip的独特特性来提高现代分析化学中的选择性，灵敏度和可持续性。

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引用次数: 0

Quantification of lactate enantiomers in human sweat samples using two-dimensional liquid chromatography 用二维液相色谱法定量测定人体汗液样品中的乳酸对映体

IF 3.2

Journal of chromatography open

Pub Date : 2025-07-21 DOI: 10.1016/j.jcoa.2025.100243

Kazushi Mori, Makoto Tsunoda

Lactate (LA) is primarily produced by the reduction of pyruvate in the human body and is crucial for energy production via anaerobic glycolysis. Although the D-LA concentration is considerably lower than that of L-LA, a significant increase in D-LA concentration alone has been reported in some diseases. Quantifying LA enantiomers in human biofluids has the potential for disease diagnosis. Sweat has recently been recognized as a novel biological alternative to blood because it can be sampled non-invasively. Therefore, in this study, heart-cutting two-dimensional liquid chromatography (2D-LC) using a highly sensitive fluorescence detection method was developed for the analysis of LA enantiomers in small amounts of human sweat. LA was derivatized with 4-nitro-7-piperazino-2,1,3-benzoxadiazole (NBD-PZ) and separated from endogenous compounds using an octadecyl silica column in the first dimension. Subsequently, the NBD-PZ-LA peak was fractionated and enantiomerically separated in the second dimension on a chiral column. Sufficient linearities (R² > 0.999) were observed in the ranges of 1–100 and 10–1000 µM for NBD-PZ-D-LA and NBD-PZ-L-LA, respectively. The corresponding limits of quantification were 0.97 and 1.12 µM. The precision values were 1.04 %–12.03 %, and the accuracies were 85.6 %–100.4 %. The developed method was successfully applied to ∼5 µL of human sweat collected from five healthy subjects. The concentrations of D-LA and L-LA in sweat were 30.29 ± 20.18 µM and 23.69 ± 12.15 mM, respectively. The developed 2D-LC system should be clinically applicable to LA enantiomer analysis in human sweat as a non-invasive biomarker.

乳酸（LA）主要由人体内丙酮酸的还原产生，对于通过厌氧糖酵解产生能量至关重要。虽然D-LA浓度明显低于L-LA，但在一些疾病中，有报道称D-LA浓度单独显著升高。定量测定人体液中的LA对映体具有疾病诊断的潜力。汗液最近被认为是血液的一种新的生物替代品，因为它可以无创取样。因此，本研究建立了采用高灵敏度荧光检测方法的切心二维液相色谱法（2D-LC），用于少量人体汗液中LA对映体的分析。LA与4-硝基-7-哌嗪基-2,1,3-苯并恶二唑（NBD-PZ）进行衍生化反应，并用十八烷基硅柱在一维上分离内源性化合物。随后，在手性柱上对NBD-PZ-LA峰进行二次分馏和对映体分离。充分的线性(R²>；NBD-PZ-D-LA和NBD-PZ-L-LA在1-100µM和10-1000µM范围内的浓度分别为0.999)。相应的定量限分别为0.97和1.12µM。精密度为1.04% ~ 12.03%，准确度为85.6% ~ 100.4%。所开发的方法成功地应用于5名健康受试者的人体汗液中。汗液中D-LA和L-LA的浓度分别为30.29±20.18µM和23.69±12.15 mM。所开发的2D-LC系统可作为无创生物标志物应用于人体汗液中的LA对映体分析。

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引用次数: 0

Critical review on the assessments of green metric tools for Olmesartan medoxomil analytical methods: Case studies 对奥美沙坦-美多索密分析方法绿色计量工具评估的批判性回顾：案例研究

Journal of chromatography open

Pub Date : 2025-07-18 DOI: 10.1016/j.jcoa.2025.100242

Shaikh Manirul Haque , Abuzar Kabir

Green chemistry metrics can incorporate features of analytical practices that adhere to the principles of green chemistry. Several metrics are available to evaluate the greenness of the analytical procedure, including the AES, AGREE, and BAGI. The current review article outlines the selected metrics used to determine case studies of Olmesartan, employing various analytical techniques, including UV spectrophotometry, HPLC, HPTLC, UPLC, LC-MS, and UPLC-MS, based on specific criteria. These criteria also include the advantages, disadvantages, and limitations of each technique. The analytical eco–scale, AGREE and BAGI values were in the range 79–86, 72–84, 66–68, 77, 75–89, 67–75; 0.6–0.71, 0.55–0.65, 0.58–0.65, 0.62, 0.65–0.66, 0.68–0.69; 77.5–82.5, 72.5–82.5; 75–77.5, 80, 75 – 80 and 80 respectively for UV spectrophotometry, HPLC, HPTLC, UPLC, LC-MS and UPLC-MS. The results are well-organised according to the criteria and have produced an excellent greener methodology. The new researchers could understand and use all the assessment tools for different purposes. Additionally, they can utilise it to develop new procedures, which could demonstrate a greener methodology for quantifying Olmesartan in various matrices.

绿色化学指标可以结合分析实践的特点，坚持绿色化学的原则。有几个指标可用于评估分析过程的环保性，包括AES、AGREE和BAGI。当前的综述文章概述了用于确定奥美沙坦案例研究的选定指标，采用各种分析技术，包括紫外分光光度法，HPLC， HPTLC， UPLC， LC-MS和UPLC- ms，基于特定标准。这些标准还包括每种技术的优点、缺点和局限性。分析生态尺度、AGREE值和BAGI值分别为79 ~ 86、72 ~ 84、66 ~ 68、77、75 ~ 89、67 ~ 75；0.6 - -0.71, 0.55 - -0.65, 0.58 - -0.65, 0.62, 0.65 - -0.66, 0.68 - -0.69;77.5 - -82.5, 72.5 - -82.5;紫外分光光度法、HPLC法、HPTLC法、UPLC法、LC-MS法和UPLC- ms法分别为75 ~ 77.5、80、75 ~ 80和80。结果是根据标准组织良好的，并产生了一个优秀的绿色方法。新的研究人员可以理解和使用所有的评估工具用于不同的目的。此外，他们可以利用它来开发新的程序，这可以展示一种更环保的方法来量化各种矩阵中的奥美沙坦。

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引用次数: 0

Ionic liquids in liquid chromatography 液相色谱中的离子液体

Journal of chromatography open

Pub Date : 2025-07-11 DOI: 10.1016/j.jcoa.2025.100239

Sini Santasalo , Susanne K. Wiedmer

The use of ionic liquids (ILs) in liquid chromatography (LC) is reviewed. ILs have several different types of functionalities, which means that they are prone to multiple simultaneous interactions with stationary phases in LC. ILs have been investigated by LC as analytes and they have been used as mobile phase additives and column stationary phase modifiers in LC. All these applications include a diverse range of interactions with different LC stationary phases. Common reasons for using ILs as mobile phase additives have been to reduce unwanted interactions between analytes and free silanols on the column stationary phase, to act as ion pair reagents to separate polar compounds with reversed phase LC, and to act as UV absorption reagents to detect compounds that do not absorb UV light. The review covers the most important works between 2003–2025.

综述了离子液体在液相色谱中的应用。l具有几种不同类型的功能，这意味着它们容易与LC中的固定相同时发生多种相互作用。液相色谱法研究了液相色谱法中液相色谱作为流动相添加剂和柱固定相改性剂的应用。所有这些应用包括与不同LC固定相的各种相互作用。使用ILs作为流动相添加剂的常见原因是为了减少色谱柱固定相上分析物与游离硅醇之间不必要的相互作用，作为离子对试剂用反相LC分离极性化合物，以及作为紫外线吸收试剂检测不吸收紫外线的化合物。该审查涵盖了2003-2025年期间最重要的工作。

引用次数: 0

A thermodynamic study of relative extractability of ethanol to blood simulating solvent in extractables and leachables analysis of medical devices by Abraham’s Solvation Parameter Model 亚伯拉罕溶剂化参数模型在医疗器械可萃取物和可浸物分析中乙醇对血液模拟溶剂相对可萃取性的热力学研究

Journal of chromatography open

Pub Date : 2025-07-11 DOI: 10.1016/j.jcoa.2025.100238

Jianwei Li

类型

全部化学•材料生命科学医学物理工程技术环境•农林材料科学地球科学法学管理学化学环境科学与生态学计算机科学教育学经济学农林科学人文科学生物学数学物理与天体物理心理学综合性期刊其他工业工程理学历史学农学文学信息工程

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