Analysis of phenylcarboxylic acid-type microbial metabolites by microextraction by packed sorbent from blood serum followed by GC–MS detection

Pautova, Alisa; Sobolev, Pavel D.; Revelsky, A. I.

doi:10.1016/j.clinms.2019.05.005

Cited by 17 publications

(9 citation statements)

References 23 publications

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“…MEPS was chosen as an alternative sample preparation method to LLE. The conditions for the extraction of the indolic acids from serum and CSF samples were based on our previous study [8] and they were significantly modified. The main modification is the reduced to 40 µL volume of the biological sample, which is important for the analysis of CSF samples.…”

Section: Analytical Characteristics Of Meps For Indolic Acid Extractionmentioning

confidence: 99%

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Determination of Tryptophan Metabolites in Serum and Cerebrospinal Fluid Samples Using Microextraction by Packed Sorbent, Silylation and GC–MS Detection

et al. 2020

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Indole-containing acids—tryptophan metabolites—found in serum and cerebrospinal fluid (CSF) samples of patients with diseases of the central nervous system (CNS) were determined with the use of microextraction by packed sorbent (MEPS) followed by silylation and gas chromatography–mass spectrometry (GC–MS) analysis. MEPS with the following silylation led to the reproducible formation of derivatives with an unsubstituted hydrogen ion in the indole ring, the chromatographic peaks of which are symmetric and can be used for GC–MS analysis without additional derivatization. The recoveries of analytes at the limit of quantitation (LOQ) levels were 40–80% for pooled CSF and 40–60% for serum. The limit of detection (LOD) and LOQ values were 0.2–0.4 and 0.4–0.5 µM, respectively, for both CSF and serum. The precision (the reproducibility, RSD) value of less than 20% and the accuracy (the relative error, RE) value of less than ±20% at the LOQ concentrations meet the Food and Drug Administration (FDA) recommendations. Linear correlations for all analytes were determined over a potentially clinically significant range of concentrations (0.4–10 µM for serum, R2 ≥ 0.9942, and 0.4–7 µM for CSF, R2 ≥ 0.9949). Moreover, MEPS significantly reduced the matrix effect of serum compared to liquid–liquid extraction (LLE), which was revealed in the example of reducing the amount of cholesterol and its relative compounds.

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Section: Analytical Characteristics Of Meps For Indolic Acid Extractionmentioning

confidence: 99%

“…Several protocols for the determination of these compounds were developed. They include liquid-liquid extraction (LLE), microextraction by packed sorbent (MEPS) with C18 and hypercrosslinked polystyrene as sorbents with the following derivatization and gas chromatography -mass spectrometry (GC-MS) analysis [7][8][9].…”

Section: Introductionmentioning

confidence: 99%

Determination of Tryptophan Metabolites in Serum and Cerebrospinal Fluid Samples Using Microextraction by Packed Sorbent, Silylation and GC–MS Detection

et al. 2020

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“…The conditions for MEPS from CSF were based on our previous study on the aromatic acid extraction from serum samples using C 18 sorbent (Pautova et al, 2019), but they were significantly modified owing to the features of the CSF. We rejected the acidification of samples and the separation of protein components by centrifugation, because CSF contains significantly less protein than blood serum.…”

Section: Application Of the Meps For Sample Pretreatmentmentioning

confidence: 99%

“…Sample preparation plays an important role in the analysis of biological fluids because of the complexity of the sample matrix. In the previous studies of our research group, protocols for determining aromatic acids in blood serum of critically ill patients using liquid–liquid extraction (LLE) and microextraction by packed sorbent (MEPS) were described (Pautova et al, 2018; Pautova, Sobolev, & Revelsky, 2019, 2020). LLE is one of the most common sample preparation techniques for extracting organic compounds from biological samples, but it has some drawbacks.…”

Section: Introductionmentioning

confidence: 99%

“…These advantages lead to a reduction of human labor input, which improves analytical productivity and reproducibility (Abdel‐Rehim, 2011; Bustamante et al, 2017). We have demonstrated that MEPS along with LLE can be used as a sample preparation method for the analysis of aromatic compounds in serum samples of both healthy people and critically ill patients and requires 2.5 times less serum volume compared with LLE (Pautova et al, 2019, 2020).…”

Section: Introductionmentioning

confidence: 99%

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Metabolic profiling of aromatic compounds in cerebrospinal fluid of neurosurgical patients using microextraction by packed sorbent and liquid–liquid extraction with gas chromatography–mass spectrometry analysis

Pautova

Khesina

Litvinova

et al. 2020

Biomedical Chromatography

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A new approach to the quantitative analysis of aromatic metabolites in cerebrospinal fluid samples of neurosurgical patients based on microextraction by packed sorbent coupled with derivatization and GC–MS was developed. Analytical characteristics such as recoveries (40–90%), limit of detection (0.1–0.3 μm) and limit of quantitation (0.4–0.7 μm) values, accuracy (<±20%), precision (<20%) and linear correlations (R2 ≥ 0.99) over a 0.4–10 μm range of concentrations demonstrated that microextraction by packed sorbent provides results for the quantitative analysis of target compounds comparable with those for liquid–liquid extraction. Similar results were achieved using 40 μl of sample for microextraction by packed sorbent instead of 200 μl for liquid–liquid extraction. Benzoic, 3‐phenylpropionic, 3‐phenyllactic, 4‐hydroxybenzoic, 2‐(4‐hydroxyphenyl)acetic, homovanillic and 3‐(4‐hydroxyphenyl)lactic acids were found in cerebrospinal fluid samples (n = 138) of neurosurgical patients in lower concentrations than in serum samples (n = 110) of critically ill patients. Analysis of the cerebrospinal fluid and serum samples taken at the same time from neurosurgical patients (n = 5) revealed similar results for patients without infection and multidirectional results for patients with central nervous system infection. Our preliminary results demonstrate the necessity of further evaluating the aromatic compound profile in cerebrospinal fluid for its subsequent verification for potential diagnostic markers.

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Recent applications of microextraction sample preparation techniques in biological samples analysis

Daryanavard

Zolfaghari

Abdel-Rehim

et al. 2021

Biomedical Chromatography

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Analysis of biological samples is affected by interfering substances with chemical properties similar to those of the target analytes, such as drugs. Biological samples such as whole blood, plasma, serum, urine and saliva must be properly processed for separation, purification, enrichment and chemical modification to meet the requirements of the analytical instruments. This causes the sample preparation stage to be of undeniable importance in the analysis of such samples through methods such as microextraction techniques. The scope of this review will cover a comprehensive summary of available literature data on microextraction techniques playing a key role for analytical purposes, methods of their implementation in common biological samples, and finally, the most recent examples of application of microextraction techniques in preconcentration of analytes from urine, blood and saliva samples. The objectives and merits of each microextration technique are carefully described in detail with respect to the nature of the biological samples. This review presents the most recent and innovative work published on microextraction application in common biological samples, mostly focused on original studies reported from 2017 to date. The main sections of this review comprise an introduction to the microextraction techniques supported by recent application studies involving quantitative and qualitative results and summaries of the most significant, recently published applications of microextracion methods in biological samples. This article considers recent applications of several microextraction techniques in the field of sample preparation for biological samples including urine, blood and saliva, with consideration for extraction techniques, sample preparation and instrumental detection systems.

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Analysis of phenylcarboxylic acid-type microbial metabolites by microextraction by packed sorbent from blood serum followed by GC–MS detection

Cited by 17 publications

References 23 publications

Determination of Tryptophan Metabolites in Serum and Cerebrospinal Fluid Samples Using Microextraction by Packed Sorbent, Silylation and GC–MS Detection

Determination of Tryptophan Metabolites in Serum and Cerebrospinal Fluid Samples Using Microextraction by Packed Sorbent, Silylation and GC–MS Detection

Metabolic profiling of aromatic compounds in cerebrospinal fluid of neurosurgical patients using microextraction by packed sorbent and liquid–liquid extraction with gas chromatography–mass spectrometry analysis

Recent applications of microextraction sample preparation techniques in biological samples analysis

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