Journal of chromatography open最新文献_第10页

Assessment of machine learning and group contribution solvation parameter model descriptors for model retention in reversed-phase liquid chromatography and gas chromatography 评估反相液相色谱和气相色谱中用于模型保留的机器学习和组贡献溶解参数模型描述符

Journal of chromatography open

Pub Date : 2025-03-13 DOI: 10.1016/j.jcoa.2025.100213

Sanka N. Atapattu , Azamat Temerdashev

Abraham's solvation parameter model is a valuable tool for modelling reversed-phase liquid chromatography and gas chromatography systems. Except for the solute descriptor McGowan's characteristic volume, V, the remaining solute descriptors E, S, A, B, and L of the solvation parameter model are experimentally determined. Estimation approaches, machine learning, and group contribution methods are two alternatives to experimental approaches to estimating solute descriptors. In this work we evaluated the applicability of solvation parameter model solute descriptors estimated using machine learning and group contribution methods. Overall solute descriptors estimated using the machine learning approach fit better than solute descriptors estimated using the group contribution method for both reversed-phase liquid chromatography and gas chromatography systems studied in this work. For the studied methanol-water binary solvent system on a Luna C18(2) stationary phase model, coefficient of determination ranged from 0.982 to 0.953 when using machine learning estimated descriptors, whereas with group contribution estimated descriptors, models ranged between 0.923 and 0.943. For the studied gas chromatography models, coefficient of determination ranged from 0.995 to 0.987 when using machine learning estimated descriptors, whereas with group contribution estimated descriptors ranged between 0.941 and 0.977. However, both machine learning and group contribution descriptors did not fit in models as well as experimentally determined reference WSU descriptors.

亚伯拉罕的溶剂化参数模型是模拟反相液相色谱和气相色谱系统的一个有价值的工具。除溶质描述子McGowan的特征体积V外，其余溶质描述子E、S、A、B和L均通过实验确定。估计方法、机器学习和群体贡献方法是估计溶质描述符的实验方法的两种替代方法。在这项工作中，我们评估了使用机器学习和群体贡献方法估计的溶剂化参数模型溶质描述符的适用性。对于本研究中研究的反相液相色谱和气相色谱系统，使用机器学习方法估计的总体溶质描述符比使用群贡献法估计的溶质描述符更适合。对于Luna C18(2)固定相模型所研究的甲醇-水二元溶剂体系，使用机器学习估计描述符时，模型的决定系数在0.982 ~ 0.953之间，而使用群体贡献估计描述符时，模型的决定系数在0.923 ~ 0.943之间。对于所研究的气相色谱模型，当使用机器学习估计描述符时，确定系数范围为0.995至0.987，而使用群体贡献估计描述符时，确定系数范围为0.941至0.977。然而，机器学习和群体贡献描述符都不适合模型以及实验确定的参考WSU描述符。

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引用次数: 0

Separation, identification, and quantification of dicyclohexylformyl oxyphenisatin, an illegal additive, from a fruit and vegetable plum 果蔬李子中非法添加剂二环己基甲酰基氧苯醌的分离、鉴定和定量

Journal of chromatography open

Pub Date : 2025-03-12 DOI: 10.1016/j.jcoa.2025.100214

Wanqin Wu , Songsong Zhu , Jintao Xia , Feng Jiang , Xiaolong Fan , Li Zhang

Purpose

This study is to develop an effective method for separating, identifying, and quantifying suspected illegal additives from fruit and vegetable plums.

Methods

Ultra performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS) was employed to perform non-targeted screening of illegal additives from more than 10 batches of fruit and vegetable plums. A diesterified oxyphenisatin analog never detected before in foodstuffs was identified from a batch of fruit and vegetable plum. This analog was separated and purified by column chromatography, and its molecular structure was analyzed and identified using one dimension and two dimension-nuclear magnetic resonance spectra (1D and 2D NMR). After obtaining the synthesized reference standard, an UPLC-PDA detection method for the quantitative analysis of this analog in real samples was established.

Results

The results showed that the characteristic fragment ions with mass/charge ratio (m/z) of 224.07 and 196.07 appeared in the MS² spectrum, indicating that the analog had the skeleton of oxyphenisatin. Combining the fitted molecular formula of suspected compound, its degree of unsaturation, and the fragment ions with mass/charge ratios of 428.18, 334.14, 83.08 in the secondary mass spectrum, we speculated that the anhydride of esterified oxyphenisatin might be cyclohexanecarboxylic anhydride, which was in good consistent with NMR spectroscopic analysis. Based on these findings, the analog was eventually named dicyclohexylformyl oxyphenisatin. UPLC-PDA test results showed that the content of this analog in a batch of fruit and vegetable plum was 614.0 mg/kg.

Conclusion

As far as we know, dicyclohexylformyl oxyphenisatin is not a food additive. Structurally, it is the product from dicyclohexylformylation of oxyphenisatin. The illegal addition of this analog to food will cause unknown harm to uninformed consumers and requires the attention of relevant departments.

目的建立一种有效的分离、鉴定和定量果蔬李子中可疑非法添加剂的方法。方法采用高效液相色谱-四极杆飞行时间质谱联用技术（UPLC-Q-TOF/MS）对10多批果蔬李子进行非靶向筛选。从一批水果和蔬菜李子中鉴定出了以前从未在食品中检测到的二酯化氧苯醌类似物。采用柱层析分离纯化该类似物，并利用一维和二维核磁共振波谱（1D和2D NMR）对其分子结构进行分析和鉴定。在得到合成的参比标准品后，建立了UPLC-PDA检测方法，用于实际样品中该类似物的定量分析。结果MS2光谱中出现质量电荷比（m/z）分别为224.07和196.07的特征片段离子，表明该类似物具有氧苯那辛的骨架。结合拟合的疑似化合物分子式、不饱和程度以及二级质谱中质荷比分别为428.18、334.14、83.08的碎片离子，推测酯化后的氧苯那汀酸酐可能为环己烷羧酸酐，与核磁共振分析结果吻合较好。基于这些发现，这种类似物最终被命名为双环己基甲酰基oxyphenisatin。UPLC-PDA试验结果表明，该类似物在一批果蔬李中的含量为614.0 mg/kg。结论就目前所知，双环己基甲酰基氧苯醌不属于食品添加剂。从结构上看，它是氧苯醌的双环己基甲酰化产物。在食品中非法添加这种类似物会对不知情的消费者造成未知的危害，需要引起有关部门的重视。

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引用次数: 0

Simultaneous determination of ceftazidime and avibactam in patients by isocratic ion-pair liquid chromatography with photometric detection 等密度离子对液相色谱-光度法同时测定头孢他啶和阿维巴坦的含量

Journal of chromatography open

Pub Date : 2025-03-11 DOI: 10.1016/j.jcoa.2025.100212

Constantin Lier , Frieder Kees , Andrea Witowski , Tim Rahmel , Steffen Pockes , Christoph Dorn

A simple and fast HPLC-UV method is described for the simultaneous determination of total or free ceftazidime and avibactam in serum, which is suitable for therapeutic drug monitoring (TDM) or pharmacokinetic studies in man. Sufficient retention of the very polar avibactam was obtained by addition of tetrabutylammonium hydrogen sulfate (TBA) as ion pairing agent, thus allowing the determination of both drugs in serum by isocratic elution. Total concentrations were determined after protein precipitation with acetonitrile, free concentrations after ultrafiltration. Separation was performed using an XBridge BEH C18 column with a mobile phase consisting of 20 mM sodium phosphate buffer/acetonitrile 90:10 (v/v), pH 6.5, containing 5 mM TBA. The lower limit of quantification was 1 mg/L for ceftazidime and 0.5 mg/L for avibactam, respectively. The imprecision of the determination of total drug was <3 %, the accuracy between 99.0 % and 104 %. Determination of free drug in quality control samples resulted in unbound fractions of 97.9 ± 2.0 % for ceftazidime and 99.4 ± 3.2 % for avibactam.

建立了同时测定血清中总头孢他啶和游离头孢他啶和阿维巴坦含量的高效液相色谱-紫外分光光度法，适用于人体治疗药物监测或药代动力学研究。通过添加四丁基硫酸氢铵（TBA）作为离子配对剂，获得极极性阿维巴坦的充分保留，从而允许用等压洗脱法测定血清中的两种药物。乙腈沉淀后测定总浓度，超滤后测定游离浓度。采用XBridge BEH C18色谱柱进行分离，流动相为20 mM磷酸钠缓冲液/乙腈90:10 (v/v), pH 6.5，含5 mM TBA。头孢他啶的定量下限为1 mg/L，阿维巴坦的定量下限为0.5 mg/L。总药含量测定的不精密度为3%，准确度在99.0% ~ 104%之间。品控样品中游离药物的测定结果表明，头孢他啶和阿维巴坦的分离率分别为97.9%±2.0%和99.4%±3.2%。

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引用次数: 0

Advanced two-dimensional liquid chromatography workflow for enhanced resolution of protein components in Indian Cobra (Naja naja) venom using hydrophobic interaction-reverse phase chromatography coupled with mass spectrometry 利用疏水相互作用-反相色谱-质谱联用技术提高印度眼镜蛇（Naja Naja）毒液中蛋白质成分分辨率的先进二维液相色谱工作流程

Journal of chromatography open

Pub Date : 2025-03-05 DOI: 10.1016/j.jcoa.2025.100211

Sunil Kumar , Kunal Krishna , Anurag S. Rathore

Snake venom exhibits complexity due to its composition of a diverse array of proteins and peptides, ranging in molecular masses from approximately 5 kDa to 200 kDa. A comprehensive understanding of the venom proteome is imperative for the design of effective therapeutic candidates. Conventional methodologies often fall short of achieving comprehensive separation of venom proteins. In the current study, we introduced a novel, online two-dimensional liquid chromatography coupled with mass spectrometry for the separation of proteins within the venom of the Indian cobra snake (Naja naja). The proposed methodology utilizes hydrophobic interaction chromatography as the first dimension and reversed-phase liquid chromatography coupled with mass spectrometry as the second dimension. Utilizing the proposed two-dimensional workflow, we successfully identified 116 proteins with the heart-cut method and 134 proteins with the comprehensive method from Naja naja venom. Notably, 18 proteins were exclusively identified with the heart-cut method, while 81 were unique to the comprehensive approach. In contrast, a standalone reverse-phase chromatography coupled with mass spectrometry method identified only 35 distinct proteins, whereas the stand-alone hydrophobic interaction chromatography method exhibited 30 distinct protein peaks. The proposed strategy offers advantages including speed (a sample run time of 45 min), detailed protein identification, and preservation of protein biological activity, particularly notable when assessing the interactions of anti-venom agents with venom components.

蛇毒由于其多种蛋白质和肽的组成而表现出复杂性，其分子质量从大约5kda到200kda不等。对毒液蛋白质组的全面了解是设计有效的候选治疗药物的必要条件。传统的方法往往无法实现毒液蛋白的全面分离。在目前的研究中，我们引入了一种新的在线二维液相色谱-质谱联用技术，用于分离印度眼镜蛇（Naja Naja）毒液中的蛋白质。该方法采用疏水相互作用色谱法作为第一维，反相液相色谱法耦合质谱法作为第二维。利用所提出的二维工作流程，我们成功地鉴定了Naja Naja毒液中的116个蛋白和134个蛋白。值得注意的是，18个蛋白被心脏切割方法独家鉴定，而81个蛋白是综合方法所特有的。相反，独立的反相色谱联用质谱法只鉴定出35种不同的蛋白质，而独立的疏水相互作用色谱法则鉴定出30种不同的蛋白质峰。该方法的优点包括速度快（样品运行时间为45分钟）、详细的蛋白质鉴定和蛋白质生物活性的保存，特别是在评估抗蛇毒剂与毒液成分的相互作用时。

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引用次数: 0

Characterization of hydrolysis products and determination of the rate of hydrolysis of Novichok A-234 in different decontaminants 诺维乔克A-234在不同去污剂中的水解产物表征及水解速率测定

Journal of chromatography open

Pub Date : 2025-03-02 DOI: 10.1016/j.jcoa.2025.100210

Cristina Youngren , Harri Kiljunen , Harri A. Heikkinen , Rahim Ullah , Susanne K. Wiedmer , Paula Vanninen

In this work, studies on the neutralization of Novichok A-234, a member of a class of nerve agents known for their high toxicity, were carried out. Three decontaminants of different composition were used; these were alkaline potassium hydroxide in ethanol, GDS-2000, and Biodecon-83, a deep eutectic solvent. After 24 and 120 h of exposure to each decontaminant, the degradation products were characterized by ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS) and UPLC-tandem MS. The rate of hydrolysis of Novichok A-234 in each decontaminant was measured using ³¹P nuclear magnetic resonance (NMR) spectroscopy. The three decontaminants showed large variations in the hydrolysis rates of Novichok A-234. The total required decontamination time until Novichok A-234 was no longer observed by ³¹P NMR, ranged from 5 to 44 h. In silico calculations were performed to predict the toxicity of the main decontamination products. All hydrolysis compounds were of lower toxicity than Novichok A-234.

在这项工作中，对诺维乔克 A-234 的中和作用进行了研究，诺维乔克 A-234 是以高毒性著称的一类神经毒剂。使用了三种不同成分的去污剂：乙醇中的碱性氢氧化钾、GDS-2000 和 Biodecon-83 （一种深共晶溶剂）。在与每种去污剂接触 24 小时和 120 小时后，降解产物通过超高效液相色谱-质谱法（UPLC-MS）和 UPLC-tandem MS 进行表征。使用 31P 核磁共振 (NMR) 光谱法测量了每种去污剂中诺维乔克 A-234 的水解速率。三种去污剂在诺维乔克 A-234 的水解率方面存在很大差异。在 31P NMR 不再观察到诺维乔克 A-234 之前所需的去污总时间从 5 到 44 小时不等。所有水解化合物的毒性都低于诺维乔克 A-234。

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引用次数: 0

Comprehensive review on chromatographic analysis of flavonoids in fruits 水果中黄酮类化合物色谱分析综述

Journal of chromatography open

Pub Date : 2025-02-19 DOI: 10.1016/j.jcoa.2025.100209

Ahmet Cetinkaya , Seyda Yayla , M. Mesud Hurkul , Sibel A. Ozkan

Flavonoids are natural compounds that are abundant in fruits and have many benefits for human health. Their antioxidant, anti-inflammatory, and anticancer effects make these compounds important for health. Chromatographic analytical methods are the most commonly used methods for detecting, separating, and quantifying flavonoids in fruit species. Methods such as high-performance liquid chromatography (HPLC), gas chromatography (GC), thin-layer chromatography (TLC), and liquid chromatography-tandem mass spectrometry (LC-MS) are crucial for the analysis of flavonoids. In recent years, hybrid systems combining MS and ultraviolet (UV) detectors have been developed to increase the sensitivity of these techniques. HPLC-MS techniques are one of the most preferred methods for determining flavonoids. Flavonoid profiles between different fruit species have been compared using this technique. Although the GC method is less widely used, it uses derivatization steps to analyze non-volatile flavonoids. The accuracy and sensitivity of GC may be limited compared to other methods. TLC, a simpler and more economical method, is still preferred for separating flavonoids. However, it is less widely used than HPLC due to its limited quantitative analysis capacity. Recently, there have been technological developments in chromatographic methods of analysis. Ultra-high-performance liquid chromatography (UHPLC) offers shorter analysis times and higher resolution, especially for separating complex flavonoid mixtures. In this review, the analysis of flavonoids using chromatographic methods and a detailed discussion of studies in the literature to determine flavonoids in fruits are discussed.

类黄酮是水果中丰富的天然化合物，对人体健康有很多好处。它们的抗氧化、抗炎和抗癌作用使这些化合物对健康很重要。色谱分析方法是检测、分离和定量水果中黄酮类化合物最常用的方法。高效液相色谱法（HPLC）、气相色谱法（GC）、薄层色谱法（TLC）和液相色谱-串联质谱法（LC-MS）是分析黄酮类化合物的重要方法。近年来，结合质谱和紫外（UV）检测器的混合系统被开发出来，以提高这些技术的灵敏度。HPLC-MS技术是测定黄酮类化合物最常用的方法之一。利用该技术比较了不同水果品种间的类黄酮谱。虽然气相色谱法应用较少，但它使用衍生化步骤来分析非挥发性黄酮类化合物。与其他方法相比，气相色谱的准确度和灵敏度可能受到限制。薄层色谱法是一种更简单、更经济的分离黄酮类化合物的方法。然而，由于其定量分析能力有限，其应用不如HPLC广泛。近年来，色谱分析方法在技术上有了很大的发展。超高效液相色谱法（UHPLC）具有分析时间短、分辨率高的特点，尤其适用于复杂类黄酮混合物的分离。本文综述了用色谱法分析水果中黄酮类化合物的研究进展，并对国内外有关测定水果中黄酮类化合物的研究进行了综述。

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引用次数: 0

Miniaturized analytical method to evaluate the profile of biogenic volatile organic compounds from Spanish tree species by gas chromatography coupled to mass spectrometry and chemometric tools 用气相色谱-质谱联用和化学计量工具评价西班牙树种生物源性挥发性有机物的小型化分析方法

Journal of chromatography open

Pub Date : 2025-02-18 DOI: 10.1016/j.jcoa.2025.100208

Adrián Fuente-Ballesteros, Ana M. Ares, José Bernal, Silvia Valverde

A novel miniaturized analytical method has been optimized to study the biogenic volatile organic compounds (BVOCs) profile from tree leaves using headspace solid-phase microextraction gas chromatography-quadrupole time-of-flight spectrometry (HS-SPME-GC-QTOF-MS). Several parameters were tested, and a 50/30 µm DVB/CAR/PDMS SPME fiber, 0.20 g of sample, extraction and desorption times of 45 and 3 mins, respectively, were selected as the optimal conditions. Subsequently, 42 samples from Ávila (Spain) were evaluated including conifers (Pinus sylvestris and Juniperus oxycedrus) and broadleaf species (Quercus ilex and Quercus pyrenaica). More than 100 different BVOCs were tentatively identified with a matching degree >85 % in the NIST library. Total compounds were categorized into 12 main groups, where sesquiterpenoids, hydrocarbons, and alcohols were the dominant family groups. Moreover, a variety of chemometric tools were applied to enable data differentiation and potential classification of samples. Principal component analysis revealed that the BVOCs produced by different tree species exhibit distinct profiles, forming three well-defined clusters, while hierarchical cluster analysis indicated that the composition is influenced by the season, and sampling height. Finally, the method was classified as environmentally friendly according to the green analytical metrics and evaluated as practical by the blue applicability grade index.

采用顶空固相微萃取气相色谱-四极杆飞行时间谱法（HS-SPME-GC-QTOF-MS）对树叶中生物源性挥发性有机物（BVOCs）进行了分析。对多个参数进行了测试，选择50/30µm DVB/CAR/PDMS SPME纤维，0.20 g样品，提取和解吸时间分别为45和3 min为最佳条件。随后，对来自Ávila （Spain）的42个样本进行了评价，包括针叶树（Pinus sylvestris和Juniperus oxycedrus）和阔叶树种（Quercus ilex和Quercus pyrenaica）。在NIST库中初步确定了100多种不同的BVOCs，匹配度为85%。总化合物分为12个主要类群，其中倍半萜类、烃类和醇类是主要的家族类。此外，还应用了各种化学计量学工具来实现数据区分和样品的潜在分类。主成分分析表明，不同树种产生的BVOCs具有明显的分布特征，形成了3个明确的聚类；层次聚类分析表明，不同树种产生的BVOCs的组成受季节和采样高度的影响。最后，根据绿色分析指标对该方法进行了环境友好分类，并通过蓝色适用性等级指数对该方法进行了实用性评价。

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引用次数: 0

Tutorial on high-performance liquid chromatography of isotopologues of organic compounds 有机化合物中同位素物的高效液相色谱分析教程

Journal of chromatography open

Pub Date : 2025-02-14 DOI: 10.1016/j.jcoa.2025.100207

P.N. Nesterenko, V.D. Kazakova

Separation of isotopologues or chemical species having different number of neutrons in one or more atoms of specific compound represents an important but difficult task. Application of high-performance liquid chromatography (HPLC) provides some flexibility in various separation modes of isotopologues via different isotopic effects. This tutorial describes basic isotopic effects (hydrophobicity, polarizability, acid-base properties, size difference, etc.), which can influence HPLC performance in the separation of isotopologues. The article is focused on separation selectivity of deuterated organic compounds, for which different properties are considered. The use of advanced adsorption materials and techniques is discussed.

在特定化合物的一个或多个原子中分离具有不同中子数的同位素或化学物质是一项重要但困难的任务。高效液相色谱（HPLC）的应用，通过不同的同位素效应，为同位素物的各种分离方式提供了一定的灵活性。本教程描述了基本的同位素效应（疏水性、极化性、酸碱性质、大小差异等），这些效应会影响HPLC分离同位素物的性能。本文主要研究了氘化有机化合物的分离选择性，考虑了不同的性质。讨论了先进吸附材料和技术的应用。

引用次数: 0

Semi-preparative on-line supercritical fluid extraction-supercritical fluid chromatography for solid-state injection and purification 半制备在线超临界流体萃取-超临界流体色谱法用于固体注射和纯化

Journal of chromatography open

Pub Date : 2025-02-06 DOI: 10.1016/j.jcoa.2025.100206

Quentin Gros, Yusuke Masuda, Yoshiyuki Watabe, Hidetoshi Terada

Thanks to the versatility and low viscosity of sub/supercritical fluids, supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) are attractive to extract and separate molecules in a quick and efficient way. By coupling both techniques, on-line SFE-SFC becomes even more versatile and can extract, separate, and detect molecules in a single approach. When used at semi-preparative (semi-prep.) scale, on-line SFE-SFC can also be an interesting tool to perform solid-state injection and simplify sample pretreatment before purification. The aim of this publication is to examine the possibilities offered by semi-prep. on-line SFE-SFC for solid-state injection and determine the key parameters for method development, using ibuprofen as a case study. First, solubility changes of ibuprofen in a pressurized carbon dioxide (CO₂)/methanol mixture were investigated, revealing a favorable solubility at 20 % of co-solvent. Then, an SFC method was developed at analytical scale and scaled up to semi-prep. SFC. This method allowed the separation of ibuprofen from structurally related compounds in less than 3 min, using a Shim-pack UC PolyVP column and 30 % of MeOH in pressurized CO₂. After that, the effect of co-solvent ratio and extraction duration on semi-prep. on-line SFE-SFC solid-state injection was investigated. With an appropriate static extraction using 20 % of co-solvent for 1 min followed by a dynamic extraction with 5 % of co-solvent over 4 min, it was possible to inject and purify 500 mg of solid-state ibuprofen in 10 min. Finally, the methodology was applied to 2.5 g of sample, demonstrating its suitability for larger solid-state injection.

由于亚/超临界流体的通用性和低粘度，超临界流体萃取（SFE）和超临界流体色谱（SFC）是一种快速有效的提取和分离分子的方法。通过结合这两种技术，在线SFE-SFC变得更加通用，可以在单一方法中提取、分离和检测分子。当用于半制备（半制备）规模时，在线SFE-SFC也可以成为进行固态进样和简化纯化前样品预处理的有趣工具。本出版物的目的是研究半准备提供的可能性。在线SFE-SFC进行固态注射并确定关键参数的方法开发，以布洛芬为例进行研究。首先，研究了布洛芬在加压二氧化碳/甲醇混合物中的溶解度变化，发现在20%的共溶剂下具有良好的溶解度。然后，在分析尺度上建立了SFC方法，并扩展到半制备。该方法使用simm -pack UC PolyVP色谱柱，在加压CO2中加入30%的MeOH，在不到3分钟的时间内将布洛芬与结构相关的化合物分离。然后考察了助溶剂比和萃取时间对半制备的影响。在线研究了SFE-SFC固态注入。用20%的共溶剂静态萃取1分钟，然后用5%的共溶剂动态萃取4分钟，可以在10分钟内注射和纯化500 mg的固体布洛芬。最后，将该方法应用于2.5 g的样品，证明了其适用于更大的固体注射。

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引用次数: 0

Evaluation of trap discs for root exudate eco-friendly sampling using rhizoboxes: Application to untargeted screening of organic compounds by gas chromatography hyphenated with high resolution mass spectrometry 利用根箱对根系分泌物进行生态友好取样的捕集盘评价：气相色谱联用高分辨率质谱法在有机化合物非靶向筛选中的应用

Journal of chromatography open

Pub Date : 2025-02-05 DOI: 10.1016/j.jcoa.2025.100205

Victoria Bohm , Estelle Forey , Matthieu Chauvat , Pascal Cardinael , Valerie Peulon-Agasse

In the present paper, an unusual sampling method, called EcoRoot, was investigated for sampling directly in soil, root exudates of Poa annua L., belonging to the Poaceae family. Using a rhizobox, sorption filters were placed directly onto roots to serve as traps for root exudates. Various trap compositions, namely, cellulose nitrate, glass microfiber and nylon, were evaluated for their ability to adsorb/desorb a standard mixture of known exuded compounds and for recovery yield. Cellulose nitrate supports exhibited better yields for compounds known to be exudated by plants of the Poaceae family. Then, two crucial parameters were investigated: the contact and extraction times. The most suitable methodology for extracting the target compounds was a cellulose nitrate support with a contact time of 60 min and 30 min in an ultrasonic bath using a mixture H₂O/MeOH. Soil and root sampling was carried out under the optimized conditions. Then, silylation of extracts was performed, and GC-HRMS was used to demonstrate that this sampling method could be used to efficiently trap compounds from soil and roots. Moreover, among the 6,136 compounds detected in extracts, 516 appeared to be specific to root exudates. This Ecoroot methodology allows root exudates to be collected in conditions as close as possible to natural growth environment, limiting the environmental impact with a 0.59 score (AGREEprep) compared to hydroponic methods. Ecoroot offers interesting perspectives for studying root exudate metabolome and their temporal and spatial dynamics in the rhizosphere, with important issues in both Ecology and Plant biology.

本文采用一种不同寻常的采样方法——EcoRoot，对禾本科植物黄花蒿（Poa annua L.）的土壤根系分泌物进行了直接采样。使用根箱，吸收过滤器直接放置在根上，作为根渗出物的陷阱。各种捕集器组合物，即硝酸纤维素、玻璃超细纤维和尼龙，被评估其吸附/解吸已知渗出化合物的标准混合物的能力和回收率。硝酸纤维素载体对已知由禾科植物渗出的化合物表现出较好的产量。然后研究了两个关键参数：接触次数和提取次数。最适合提取目标化合物的方法是硝酸纤维素载体，使用H2O/MeOH混合物在超声波浴中接触时间为60 min和30 min。在优化条件下进行土壤和根系取样。然后，对提取物进行硅基化处理，并使用GC-HRMS证明该采样方法可以有效地捕获土壤和根系中的化合物。此外，在提取物中检测到的6136种化合物中，516种似乎对根渗出液有特异性。这种Ecoroot方法允许在尽可能接近自然生长环境的条件下收集根分泌物，与水培方法相比，将环境影响限制在0.59分（AGREEprep）。Ecoroot为研究根际分泌物代谢组及其时空动态提供了有趣的视角，在生态学和植物生物学中具有重要意义。

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引用次数: 0