Packed-fiber Solid-phase Extraction Research Articles

A novel extraction method for three ochratoxins in human urine based on polystyrene/polyethersulfone electrospun nanofibers coated with copper nanoparticles.

In this study, four types of nanofibers were prepared via electrospinning and characterized through SEM, TEM, EDS, FTIR, TG, XPS and water contact angle analyses, and the novel polystyrene/polyethersulfone nanofibers coated with copper nanoparticles (PS/PES-CuNPs nanofibers) were developed as an ideal adsorbent for the extraction of three ochratoxins from human urine. The solid-phase extractant of sample pretreatment displayed preferable sensitivity and an extraction effect, and the analytical method based on the novel packed-fiber solid-phase extraction strategy followed by high performance liquid chromatography-fluorescence detection (PFSPE-HPLC-FLD) achieved an exceedingly low limit of detection (LOD) and limit of quantification (LOQ) of 0.108-0.162 μg L-1 and 0.658-0.701 μg L-1, respectively; a high spiked recovery of 71.3-92.0% and a lower adsorption time of 7 min, thus demonstrating excellent results compared with other reported adsorbents for ochratoxins from various samples. With the application of this method for the detection of ochratoxins in human urine samples, six in thirty samples were tested positive. This study confirmed that the PS/PES-CuNP nanofibers and PFSPE showed promising potential as a sensitive method for simultaneous extraction and detection of ochratoxins in complex samples.

Determination of polyamines in urine via electrospun nanofibers-based solid-phase extraction coupled with GC-MS and application to gastric cancer patients.

The simultaneous determination of polyamines and their metabolites in urine samples was achieved by gas chromatography-mass spectrometry in the selected ion monitoring mode. After conjugating with the ion-pair reagent bis-2-ethylhexylphosphate in the aqueous phase, the polyamines in the samples were extracted with polystyrene nanofiber-based packed-fiber solid-phase extraction followed by a derivatization step using pentafluoropropionyl anhydride. With optimal conditions, all analytes were separated well. For analytes of putrescine, cadaverine, N-acetylputrescine, and N-acetylcadaverine, the linearity was good in the range of 0.05-500 μmol/L (R2 ≥0.993). While for spermidine, spermine, acetylspermidine, N8 -acetylspermidine, and N-acetylspermine, the linearity was good in the range of 0.5-500μmol/L (R2 ≥0.990). The recoveries of three spiked concentrations (0.5, 5, 300μmol/L) were 85.6%-108.4%, and relative standard deviations for intra- and interday were in the range of 2.9%-13.4% and 4.5%-15.1%, respectively. The method was successfully applied to the analysis of urine samples of gastric cancer patients. The results showed that the levels of most polyamines and N-acetylated polyamines from the patient group were significantly higher than those from the control group. The altered concentrations of the above-mentioned metabolites suggest their role in the pathogenesis of gastric cancer, and they should be further evaluated as potential markers of gastric cancer.

Electrospun Polycrown Ether Composite Nanofibers as an Adsorbent for On-Line Solid Phase Extraction of Eight Bisphenols from Drinking Water Samples with Column-Switching Prior to High Performance Liquid Chromatography.

Bisphenols (BPs) are a class of endocrine disruptors widely existing in the environment. They have a great impact on human health owing to their environmental endocrine disrupting effects, chronic toxicity, neurotoxicity, cytotoxicity and genetic toxicity. In this paper, an on-line packed fiber solid phase extraction (PFSPE) coupling with column-switching HPLC-FLD determination method was developed for the determination of eight BPs in drinking water. The poly (dibenzo-18-crown-6-ether)/polystyrene composite nanofibers (PDB18C6/PS) were prepared by electrospinning and used as an adsorbent for the on-line PFSPE column. The on-line PFSPE-HPLC equipment contained a dual ternary pump and a switching valve to enable enrichment, purification, and analysis directly in the system. The results showed that the proposed on-line PFSPE-HPLC-FLD method realized the simultaneous separation and detection of eight BPs: BPF, BPE, BPA, BPB, BPAF, BPAP, BPC and BPZ. The curves of the target analytes were prepared with good correlation coefficient values (r2 > 0.998) in the range of 50-1000 pg/mL. The limit of detection (S/N = 3) was 20 pg/mL, the limit of quantitation (S/N = 10) is 50 pg/mL. The recoveries of eight BPs were 94.8-127.3%, and the intra-day precisions (RSD) were less than 10%. The PFSPE column made of the PDB18C6/PS composite nanofibers has stable properties and can be reused at least 200 times. In the detection of drinking water samples, BPZ was detected in nearly 80% of drinking water samples, and BPA, BPAP, BPF and BPAF were also detected in some water samples. This high level of integration and automation was achieved in pretreatment of eight BPs from water samples. The proposed simple, rapid, and practical method has been successfully applied to the detection of eight BPs in drinking water, which can provide powerful technical support for drinking water quality and safety monitoring.

Composite Nanofibers as Novel Sorbents for On-Line and Off-Line Solid-Phase Extraction in Chromatographic System: A Comparison for Detection of Free Biogenic Monoamines and Their Metabolites in Plasma.

Two different pretreatment approaches have been used for the enrichment and separation of biogenic monoamines and metabolites in plasma for high performance liquid chromatography (HPLC) determination. The first approach, based on on-line packed-fiber solid-phase extraction (PFSPE) coupled with HPLC, allows for the simultaneous detection of epinephrine (E), norepinephrine (NE), dopamine (DA), 3-methoxyl epinephrine (MN), norepinephrine (NMN), 3-methoxytyramine (3-MT), and 5-hydroxytryptamin (5-HT). Using this developed on-line PFSPE–HPLC method, the limit of detections (LODs) of the seven analytes ranged from 1 ng/mL (NMN and MN) to 2 ng/mL (NE, E, DA, 3-MT and 5-HT). The reportable ranges were 5–300 ng/mL for NE and DA, 5–100 ng/mL for E, and 5–200 ng/mL for NMN, MN, 3-MT and 5-HT. The off-line PFSPE–HPLC was employed in the second approach and could provide simultaneous detection of NE, E, DA, NMN, and MN. The linearity was verified in the range of 0.5–20 ng/mL (NE, E, and DA) and 20–250 ng/mL (NMN and MN). The LODs of the five analytes ranged from 0.2 ng/mL (NE, E, and DA) to 5 ng/mL (NMN and MN). This study verified the possibility of using nanofibers as an adsorbent in an on-line PFSPE–HPLC system for the determination of biogenic monoamines and their metabolites in human plasma. Compared with the off-line PFSPE approach, the on-line PFSPE method deserves attention mainly due to its greener character, derived from the automation of the process and high-throughput with less operators’ handling.

Packed-Fiber Solid Phase-Extraction Coupled with HPLC-MS/MS for Rapid Determination of Lipid Oxidative Damage Biomarker 8-Iso-Prostaglandin F2α in Urine.

The 8-iso-prostaglandin F2α (8-iso-PGF2α) biomarker is used as the gold standard for tracing lipid oxidative stress in vivo. The analysis of urinary 8-iso-PGF2α is challenging when dealing with trace amounts of 8-iso-PGF2α and the complexity of urine matrixes. A packed-fiber solid-phase extraction (PFSPE)–coupled with HPLC-MS/MS–method, based on polystyrene (PS)-electrospun nanofibers, was developed for the specific determination of 8-iso-PGF2α in urine and compared with other newly developed LC-MS/MS methods. The method, which simultaneously processed 12 samples within 5 min on a self-made semi-automatic array solid-phase extraction processor, was the first to introduce PS-electrospun nanofibers as an adsorbent for the extraction of 8-iso-PGF2α and was successfully applied to real urine samples. After optimizing the PFSPE conditions, good linearity in the range of 0.05–5 ng/mL with R2 > 0.9996 and a satisfactory limit of detection of 0.015 ng/mL were obtained, with good intraday and interday precision (RSD < 10%) and recoveries of 95.3–103.8%. This feasible method is expected to be used for the batch quantitative analysis of urinary 8-iso-PGF2α.

Simultaneous Determination of Nine Quinolones in Pure Milk Using PFSPE-HPLC-MS/MS with PS-PAN Nanofibers as a Sorbent.

In this study, a packed-fiber solid-phase extraction (PFSPE)-based method was developed to simultaneously detect nine quinolones, including enrofloxacin (ENR), ciprofloxacin (CIP), ofloxacin (OFL), pefloxacin (PEF), lomefloxacin (LOM), norfloxacin (NOR), sarafloxacin (SAR), danofloxacin (DAN), and difloxacin (DIF), in pure milk, using high-performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). Polystyrene (PS) and polyacrylonitrile (PAN) were combined to form PS-PAN composite nanofibers through electrospinning. The nanofibers were used to prepare the home-made extraction columns, and the process was optimized and validated using blank pure milk. The analytical method showed high accuracy, and the recoveries were 88.68–97.63%. Intra-day and inter-day relative standard deviations were in the ranges of 1.11–6.77% and 2.26–7.17%, respectively. In addition, the developed method showed good linearity (R2 ≥ 0.995) and low method quantification limits for the nine quinolones (between 1.0–100 ng/mL) for all samples studied. The nine quinolones in the complex matrix were directly extracted using 4.0 mg of PS-PAN composite nanofibers as a sorbent and completely eluted in 100 μL elution solvent. Therefore, the developed PFSPE-HPLC-MS/MS is a sensitive and cost-effective technique that can effectively detect and control nine quinolones in dairy products.

Sampling and concentration of particulate matter bound polycyclic aromatic hydrocarbons (PAHs) basing on polystyrene nanofibers followed a determination by gas chromatography-mass spectrometry

Electrospun polystyrene (PS) nanofibers as an effective particulate filter and a sorbent in a packed-fiber solid phase extraction (PFSPE) were used to develop a novel method for the sampling and concentration of sixteen polycyclic aromatic hydrocarbons (PAHs) in the atmospheric particulate matter (PM). The PAHs were quantified by gas-chromatography-mass spectrometry (GC–MS). The main factors (the shape of PFSPE devices, the leaching solvents, and the elution methods) affecting the adsorption and desorption of PAHs on PS nanofibers were evaluated in detail. Under the optimized conditions (sampling of particulate matter bound PAHs basing on PS nanofibers filter following the release of them with ultrsound for 20 min in ethanol, the concentration of PAHs by adsorption of them on PS nanofibers again in a disk PFSPE-column, eluting of PAHs in ethanol at 75 ○C for 10 min), PS nanofibers displayed excellent properties in the sampling of PM bound PAHs and in the concentration of PAHs in the leaching solution with the recoveries ranging from 79.2 to 104.5%. The linear calibration curves were in the range of 0.17 to 64.9 ng m−3, and relative standard deviations (RSDs) were 3.8–11.6% for intra-day, 4.3–10.2% for inter-day. The method was fast, sensitive, cost-effective, with less harmful reagents, and has great potential for analyzing PAHs in atmospheric particulate matter.

Determination of three urinary catecholamines and serotonin by on-line packed-fiber solid-phase extraction

生物单胺包括儿茶酚胺类以及5-羟色胺等,在中枢神经系统中扮演着非常关键的角色,也是临床上诊断神经内分泌肿瘤疾病的重要生物标志物。由于这类单胺类物质的强化学极性导致传统吸附材料对其吸附效果不佳,从复杂生物样本中同时检测更多的生物单胺存在挑战性。该文建立了一种基于聚冠醚纳米纤维在线固相萃取检测尿液中3种儿茶酚胺(多巴胺、肾上腺素、去甲肾上腺素)和5-羟色胺的方法。采用静电纺丝法制备聚二苯并-18-冠-6醚-聚苯乙烯复合纳米纤维(PCE-PS),制成装填纤维的固相萃取(PFSPE)柱,再将PFSPE柱与HPLC进行在线联用。该在线PFSPE-HPLC方法采用双三元泵进行样品富集净化和分析,左泵连接PFSPE柱,进行样品富集净化;右泵连接分析柱进行样品分离检测。控制切换阀的切换,实现样品富集后洗脱至分析柱中分离检测。结果表明,在线PFSPE-HPLC检测尿液儿茶酚胺(多巴胺、肾上腺素、去甲肾上腺素)和5-羟色胺在1~200 ng/mL范围内有良好的线性关系,线性相关系数达0.996以上。3种儿茶酚胺和5-羟色胺的检出限(S/N=3)分别为1和2.5 ng/mL,定量限(S/N=10)分别为2.5和5 ng/mL。空白尿液和实际尿液加标回收率在83.5%~117.7%之间,日内精密度<10%。PCE-PS复合纳米纤维在多次使用后无明显变化,具有良好的稳定性,可重复使用达95次以上。在线PFSPE-HPLC方法能够集样品在线前处理与分析检测于一体,省时省力,实现分析过程的高度自动化。该方法成功应用于尿液中3种儿茶酚胺和5-羟色胺的检测,可以为临床上相关疾病检测诊断和研究提供有力的技术支持。

Rapid determination of seven synthetic dyes in casual snacks based on packed-fibers solid-phase extraction coupled with HPLC-DAD

Based on packed-fiber solid-phase extraction and HPLC-DAD, a simple analytical method for the determination of seven synthetic dyes has been successfully developed. Polystyrene/polypyrrole (PS/PPy) fibers were obtained via electro-spinning of polystyrene skeletal nanofibers, followed by the oxidation with FeCl3 to trigger the polymerization of pyrrole and the deposition of polypyrrole coatings on PS fibrous skeleton fibers. The relationship between the extraction performance of the fibers and the electrospinning process at different humidities was investigated based on morphologic study and BET surface area. In the extraction process, purification, concentration, and desorption could be accomplished in one step. The established method exhibited good sensitivity, selectivity, reproducibility, and good efficiency for synthetic dyes in casual snacks (preserved fruit, flavored yogurt, and fruity hard candy) samples. With optimal conditions, the LODs (S/N = 3) were 2.4 to 21.09 ng mL−1, and linearities were acceptable in liquid matrix and solid matrices. The recoveries were 93.9–103.9%.

Simultaneous analysis of two urinary biomarkers of oxidative damage to DNA and RNA based on packed-fiber solid phase extraction coupled with high-performance liquid chromatography

The determination of the concentrations of urinary biomarkers of oxidative damage to DNA and RNA is difficult due to the low content of targets and the complex matrix of urine. A method using polystyrene/polypyrrole (PS/PPY) electronspun nanofibers as the adsorbent was introduced to the routine urinary treatment and determination of 8-OHdG and 8-oxoG for the first time. And 2-aminoethyl diphenylborate (DPBA) solution was creatively used in the loading and rinsing steps in order to promote the retention of the analytes as well as remove impurities. Under optimal conditions, 8-OHdG, 8-oxoG and IS were separated very well and exhibited a good linearity in the range of 0.5–50 ng mL−1, with correlation coefficients of R2 > 0.996. Limits of detection (LOD) were 0.058 ng mL−1 and 0.093 ng mL−1, and limits of quantification (LOQ) were 0.195 ng mL−1 and 0.309 ng mL−1, respectively. The recoveries were 88.8–104.9%. The proposed method was so simple and economical that it had the potential to be applied to batch quantitative analysis of 8-OHdG and 8-oxoG in urine. And it was successfully applied to real urine samples of cancer patients.

Automated on-line packed fiber solid phase extraction for determination of urinary catecholamines

Despite the development of an off-line packed fiber solid phase extraction procedure (PFSPE) for urinary catecholamines, automation remains a challenge. Here, we propose an on-line PFSPE-HPLC procedure for automated sample processing and analysis of urinary catecholamines, with good recovery and precision, to avoid manual operation errors. The on-line PFSPE-HPLC procedure has been thoroughly optimized concerning the gradient, valve switch timing, the effects of complexing reagent and buffer solution, and the stability of the nanofibers. Validation of the developed on-line PFSPE-HPLC protocol in urine yielded satisfactory accuracies of 99.6–104.2%, precision below 7.0%, as well as a linear range from 1 ng/mL to 100 ng/mL with a correlation coefficient of 0.999. The developed protocol is herein presented as a potential technology for automated sample pretreatment for the determination of urinary catecholamines.

Rapid Determination of Vitamins D2 and D3 in Dairy Products by High‑Performance Liquid Chromatography after Solid Phase Extraction Based on Polystyrene/Polypyrrole Composite Nanofibers

The detection of vitamin D in complex samples is challenging because of the instability of vitamin D in sample preparation. To resolve this problem, packed-fiber solid-phase extraction (PFSPE) has been successfully developed for the pre-treatment of samples containing vitamin D2 (D2) and vitamin D3 (D3) in dairy products. Based on PFSPE, vitamin D could avoid oxidation because of the shorter extraction time. The adsorbent materials, polystyrene/polypyrrole (PS/PPy) nanofibers, were prepared by electrospinning of PS and in situ polymerization of PPy on the surface of PS nanofibers. The linearity was within the range of 1-2000 ng mL−1 in dairy solution, and the recoveries were 91.9-109.1% with a relative standard deviation (RSD) < 13.6%. Therefore, the prepared method could be used for the detection of D2 and D3 in dairy products.

Solid phase extraction with Polypyrrole nanofibers for simultaneously determination of three water-soluble vitamins in urine

This paper put forward a prospective pre-cleanup method of packed-fiber solid phase extraction by using Polypyrrole (Ppy) electrospun nanofibers as the sorbent to simultaneously extract three water-soluble vitamins (i.e., folic acid, cyanocobalamin and riboflavin) in human urine. Primary extraction of target analytes was carried out by loading samples onto the column along with diphenylboronic acid 2-aminoethylester (DPBA) reagent, and then the column should be rinsed with DPBA solution for three times before eluting. The DPBA was innovatively applied as complexing reagent to retain as much of three analytes as possible on the column based on the multi interaction between three vitamins and the boronate affinity reagent, thus improving hydrophobicity of targets and adsorption efficiency through loading and rinsing steps. Under optimized conditions, sample concentration factor was five times with small amount of organic solvent consumed and recoveries between 84.9% to 125.4%, and the lowest detection limit (LOD) between 0.020 to 0.041 μg/mL were achieved. Finally, the urine samples from a group of healthy children were processed with the optimized method. It proved that the proposed method is applicable in the determination of urinary B-vitamins in big samples of people.

Improved Sample Preparation Using Packed-Fiber Solid Phase Extraction in the Determination of Urinary P-Cresol

Improved Sample Preparation Using Packed-Fiber Solid Phase Extraction in the Determination of Urinary P-Cresol

High-throughput and selective solid-phase extraction of urinary catecholamines by crown ether-modified resin composite fiber

In the present study, we developed a simple and high-throughput solid phase extraction (SPE) procedure for selective extraction of catecholamines (CAs) in urine samples. The SPE adsorbents were electrospun composite fibers functionalized with 4-carboxybenzo-18-crown-6 ether modified XAD resin and polystyrene, which were packed into 96-well columns and used for high-throughput selective extraction of CAs in healthy human urine samples. Moreover, the extraction efficiency of packed-fiber SPE (PFSPE) was examined by high performance liquid chromatography coupled with fluorescence detector. The parameters affecting the extraction efficiency and impurity removal efficiency were optimized, and good linearity ranging from 0.5 to 400 ng/mL was obtained with a low limit of detection (LOD, 0.2–0.5 ng/mL) and a good repeatability (2.7%–3.7%, n = 6). The extraction recoveries of three CAs ranged from 70.5% to 119.5%. Furthermore, stable and reliable results obtained by the fluorescence detector were superior to those obtained by the electrochemical detector. Collectively, PFSPE coupled with 96-well columns was a simple, rapid, selective, high-throughput and cost-efficient method, and the proposed method could be applied in clinical chemistry.

A Convenient Method for Extraction and Analysis with High-Pressure Liquid Chromatography of Catecholamine Neurotransmitters and Their Metabolites.

The extraction and analysis of catecholamine neurotransmitters in biological fluids is of great importance in assessing nervous system function and related diseases, but their precise measurement is still a challenge. Many protocols have been described for neurotransmitter measurement by a variety of instruments, including high-pressure liquid chromatography (HPLC). However, there are shortcomings, such as complicated operation or hard-to-detect multiple targets, which cannot be avoided, and presently, the dominant analysis technique is still HPLC coupled with sensitive electrochemical or fluorimetric detection, due to its high sensitivity and good selectivity. Here, a detailed protocol is described for the pretreatment and detection of catecholamines with high pressure liquid chromatography with electrochemical detection (HPLC-ECD) in real urine samples of infants, using electrospun composite nanofibers composed of polymeric crown ether with polystyrene as adsorbent, also known as the packed-fiber solid phase extraction (PFSPE) method. We show how urine samples can be easily precleaned by a nanofiber-packed solid phase column, and how the analytes in the sample can be rapidly enriched, desorbed, and detected on an ECD system. PFSPE greatly simplifies the pretreatment procedures for biological samples, allowing for decreased time, expense, and reduction of the loss of targets. Overall, this work illustrates a simple and convenient protocol for solid-phase extraction coupled to an HPLC-ECD system for simultaneous determination of three monoamine neurotransmitters (norepinephrine (NE), epinephrine (E), dopamine (DA)) and two of their metabolites (3-methoxy-4-hydroxyphenylglycol (MHPG) and 3,4-dihydroxy-phenylacetic acid (DOPAC)) in infants' urine. The established protocol was applied to assess the differences of urinary catecholamines and their metabolites between high-risk infants with perinatal brain damage and healthy controls. Comparative analysis revealed a significant difference in urinary MHPG between the two groups, indicating that the catecholamine metabolites may be an important candidate marker for early diagnosis of cases at risk for brain damage in infants.

Solid-Phase Extraction with Packed-Fiber is a Biological Sample Preparation Tool for Neuro-Active Molecule Detection.

Neurotransmitters play a major role in shaping everyday life and functions. Accurate analytical methods are needed for detection of neurotransmitters. Packed-fiber solid-phase extraction (PFSPE) has been developed and seems to be an efficient method. This novel method is based on use of an electrospun polymer device, based on nanofibers. This strategy will be helpful for the development of real-time methods and techniques with high sensitivity to detect target neurotransmitters with high efficiency. Here we provide a brief overview of PFSPE and its applications for the determination of neuro-active molecules.

Packed-Nanofiber solid phase extraction coupled with gas chromatography-mass spectrometry for the determination of phthalate esters in urines from children.

In this paper, we developed a rapid and safe method based on packed-fiber solid-phase extraction (PFSPE) system coupled with gas chromatography-mass spectrometry for the determination of four phthalate esters (PAEs), diethyl-o-phthalate (DEP), dibutyl-o-phthalate (DBP), di (2-ethylhexyl) phathalate (DEHP), di-n-octyl phthalate (DNOP), in urine samples. The PAEs in urine samples (500μL) were rapidly cleaned up from urines using polystyrene (PS) nanofibers packed micro-columns fitted on a PFSPE pretreatment device, which can process up to 12 samples simultaneously in 5min. Under optimum conditions, satisfied recovery and relative standard deviation values (RSDs) were in the range of 80.4-111.7% and 1.5-10.9%, respectively. The limits of detection (LOD) and the limits of quantification (LOQ) were ranged from 0.1 to 0.5ngmL-1 and 0.5-2ngmL-1, respectively. The well controlled matrix effect was also evaluated by comparing the signal response of the pure PAEs standards dissolved in methanol with the signal response of PAEs in the urine matrix. This new method was successfully applied to determine four PAEs in urine samples of overweight and normal-weight children, and an association between phthalates in urines and obesity was observed. Thus, the method seems to be a useful tool for monitoring of the level of urinary phthalate esters and also to support an evidence for further reasearch of obesity.

Simultaneous quantification of cortisol and cortisone in urines from infants with packed-fiber solid-phase extraction coupled to HPLC-MS/MS.

Cortisol and cortisone are two important glucocorticoids in human body, their interconversion is controlled by two isotypes of 11β-hydroxy steroid dehydrogenase (11β-HSD1 and 11β-HSD2). The ratio of urinary cortisol to cortisone can be used to assess the activity of 11β-HSDs. An analytical method to quantify urinary cortisol and cortisone using high performance liquid chromatographic tandem mass spectrometry following a packed-fiber solid-phase extraction (PFSPE) was developed. The proposed method was validated and applied to determine the urinary cortisol and cortisone concentrations in infants. Linearity was observed in the range of 0.6-150ng/mL for cortisol and 0.8-200ng/mL for cortisone. The intra-day RSD was 2.4-4.5% for cortisol and 3.3-6.2% for cortisone. Inter-day RSD was 3.7-6.6% for cortisol and 4.3-8.2% for cortisone. The recovery was 97.8±4.6% for cortisol and 98.9±4.4% for cortisone. The established method is simple and efficient for the quantification of urinary cortisol and cortisone and for indirectly assessing the activity of 11β-hydroxy steroid dehydrogenase.

Application of packed-fiber solid-phase extraction coupled with GC–MS for the determination of short-chain fatty acids in children's urine

BackgroundAutism spectrum disorder (ASD) is a complex disorder involving interactions between genetic, epigenetic and environmental factors. Gastrointestinal (GI) disorders are prevalent in the cohort of children with ASD and they have been recognized as a comorbid condition recently. It is of value to monitor GI issues in individuals, and to help further characterize factors that may contribute to GI disorders (in individuals with and without ASD). Due to the biological relevance of short-chain fatty acids (SCFAs) to GI disorders, it is important to develop a rapid and selective detection method capable of identifying and quantifying SCFAs in complex biological samples. Because of low concentration and hydrophilicity of SCFAs, the pretreatment of sample becomes the key step to detection method. We erected and verified a packed-fiber solid-phase extraction (PFSPE) based on Polypyrrole (PPY) nanofibers coupled with gas chromatography–mass spectrometry (GC–MS) to determine SCFAs in urine. The proposed method was applied to detect SCFAs in urine from children with and without ASD, and the results between the 2 groups was compared. MethodsPFSPE method was utilized for the direct pretreatment of SCFAs in urine from children. The SCFAs extracted on nanofibers was subsequently eluted with hydrochloric acid ethanol solution and detected by GC–MS. ResultsIntraday and interday assay CVs were ≤10%, and the recoveries was 82.6%–110.5%. Limit of detection (LOD) and limit of quantification (LOQ) were 0.25–2.67ng/ml and 0.85–8.97ng/ml, respectively. The level of SCFAs in urine from children with ASD were significantly higher than that from control group. ConclusionThe proposed method improves the simplification of sample treatment and displays sufficient analytical sensitivity and selectivity. The assay offers a potential to monitor the SCFAs in urine in clinical and experimental investigation of ASD.