scholarly journals Identification of Six Phytochemical Compounds from Asparagus officinalis L. Root Cultivars from New Zealand and China Using UAE-SPE-UPLC-MS/MS: Effects of Extracts on H2O2-Induced Oxidative Stress

Nutrients ◽  
2019 ◽  
Vol 11 (1) ◽  
pp. 107 ◽  
Author(s):  
Hongxia Zhang ◽  
John Birch ◽  
Jinjin Pei ◽  
Isam A. Mohamed Ahmed ◽  
Haiyan Yang ◽  
...  
Keyword(s):  
Oxidative Stress ◽  
New Zealand ◽  
Ferulic Acid ◽  
Caffeic Acid ◽  
Bioactive Compounds ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Asparagus Officinalis ◽  
Commercial Application ◽  
Relative Standard

A simple, rapid, specific, and sensitive method was developed for the simultaneous identification and quantification of six major bioactive compounds, namely, caffeic acid, quercetin, apigenin, ferulic acid, baicalein, and kaempferol, from Asparagus officinalis roots (ARs) native to New Zealand (green and purple cultivars) and China (yellow, green, purple, and white cultivars) using ultrasound-assisted, solid-phase extraction (UASE-SPE) coupled with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The method was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy (expressed as recovery %), and precision (expressed as relative standard deviation (%RSD)). The retention times, ultraviolet visible (UV-vis) data, and mass spectral patterns of the detected peaks matched those of commercial standards, allowing characterization of the target compounds. The LODs and LOQs were 23 ng/mL and 70 ng/mL, 50 ng/mL and 150 ng/mL, 10 ng/mL and 30 ng/mL, 18 ng/mL and 54 ng/mL, 14.4 ng/mL and 43.6 ng/mL, and 7.5 ng/mL and 22.5 ng/mL for caffeic acid, quercetin, apigenin, ferulic acid, baicalein, and kaempferol, respectively, and the mean recovery rates were 85.8%, 73.0%, 90.2%, 80.6%, 76.7%, and 74.5% for the six compounds, respectively. The levels of the target compounds were significantly different (p < 0.05) among the six cultivars. The Chinese yellow AR had the highest levels of bioactive compounds: 6.0, 3.9, 0.4, 1.0, 0.86, and 0.8 mg/g for caffeic acid, quercetin, apigenin, ferulic acid, baicalein, and kaempferol, respectively. The AR extracts showed protective effects against oxidative stress in the HepG2 and L929 cell lines. The results indicate that AR extracts contain high flavonoid levels that provide protective functions against oxidative stress and support the potential commercial application of AR extracts.

scholarly journals Determination of Organic Acids in Salicornia herbacea by Solid-phase Extraction Combined with Liquid Chromatography

2013 ◽  
Vol 8 (2) ◽  
pp. 1934578X1300800
Author(s):  
Damian Han ◽  
Minglei Tian ◽  
Dong Wha Park ◽  
Kyung Ho Row
Keyword(s):  
Solid Phase Extraction ◽  
Ferulic Acid ◽  
Caffeic Acid ◽  
Solid Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Trifluoracetic Acid ◽  
Spe Method ◽  
Salicornia Herbacea

A solid-phase extraction (SPE) method for the determination of procatechuic acid, ferulic acid and caffeic acid in Salicornia herbacea L. (Hamcho) has been developed. The optimal conditions were obtained by using a C18 SPE cartridge. By using ethanol and acetonitrile /water/ trifluoracetic acid as washing and eluting solvents, most interfering compounds originating from the hamcho matrix were eliminated. The extracts were sufficiently clean to be directly injected into the HPLC for further chromatographic analysis. Good linearity was obtained from 0.1 to 200 μg/mL (r > 0.999) for procatechuic acid, 0.2 to 400 μg/mL (r > 0.999) for caffeic acid and 0.3 to 600 μg/mL (r > 0.999) for ferulic acid, with the relative standard deviations being less than 3.6%. The mean recoveries of procatechuic acid, ferulic acid and caffeic acid from hamcho were more than 79.2% and the detection limit (S/N = 3:1) was 0.02 μg/mL for procatechuic acid, 0.01 μg/mL for caffeic acid and 0.04 μg/mL for ferulic acid. This method is a viable alternative to the existing HPLC methods for analyzing the content of procatechuic acid, ferulic acid and caffeic acid in hamcho.

Calcium/Copper alginate framework doped with CuO nano-particles as a novel adsorbent for micro-extraction of benzodiazepines from human serum

2020 ◽  
Vol 16 ◽  
Author(s):  
Nadereh Rahbar ◽  
Fatemeh Ahmadi ◽  
Zahra Ramezani ◽  
Masoumeh Nourani
Keyword(s):  
Human Serum ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Nano Particles ◽  
Limit Of Quantification ◽  
Analytical Methodology ◽  
Fiber Fabrication ◽  
Relative Standard ◽  
Green Procedure

Background: Sample preparation is one of the most challenging phases in pharmaceutical analysis, especially in biological matrices, affecting the whole analytical methodology. Objective: In this study, a new Ca(II)/Cu(II)/alginate/CuO nanoparticles hydrogel fiber (CCACHF) was synthesized through a simple, green procedure and applied for fiber micro solid phase extraction (FMSPE) of diazepam (DIZ) and oxazepam (OXZ) as model drugs prior to high-performance liquid chromatography-UV detection (HPLC-UV). Methods: Composition and morphology of the prepared fiber were characterized and the effect of main parameters on the fiber fabrication and extraction efficiency have been studied and optimized. Results: In optimal conditions, calibration curves were linear ranging between 0.1–500 µg L−1 with regression coefficients of 0.9938 and 0.9968. Limit of detection (LOD) (S/N=3) and limit of quantification (LOQ) (S/N=10) of the technique for DIZ and OXZ were 0.03 to 0.1 µg L−1. Within-day and between-day relative standard deviations (RSDs) for DIZ and OXZ were 6.0–12.5% and 3.3–9.4%, respectively. Conclusion: The fabricated adsorbent has been substantially employed to extraction of selected benzo-diazepines (BZDs) from human serum real specimens and the obtained recoveries were also satisfactory (82.1-109.7%).

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

Flow-Through Fourier Transform Infrared Sensor for Total Hydrocarbons Determination in Water

2009 ◽  
Vol 63 (9) ◽  
pp. 1015-1021 ◽  
Author(s):  
David Pérez-Palacios ◽  
Sergio Armenta ◽  
Bernhard Lendl
Keyword(s):  
Fourier Transform ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Chlorinated Solvents ◽  
Analytical Signal ◽  
Fourier Transform Infrared ◽  
Minimal Sample ◽  
Relative Standard ◽  
Ft Ir ◽  
Flow Through

A new flow-through Fourier transform infrared (FT-IR) sensor for oil in water analysis based on solid-phase spectroscopy on octadecyl (C18) silica particles has been developed. The C18 non-polar sorbent is placed inside the sensor and is able to retain hydrocarbons from water samples. The system does not require the use of chlorinated solvents, reducing the environmental impact, and the minimal sample handling stages serve to ensure sample integrity whilst reducing exposure of the analyst to any toxic hydrocarbons present within the samples. Fourier transform infrared (FT-IR) spectra were recorded by co-adding 32 scans at a resolution of 4 cm−1 and the band located at 1462 cm−1 due to the CH2 bending was integrated from 1475 to 1450 cm−1 using a baseline correction established between 1485 and 1440 cm−1 using the areas as analytical signal. The technique, which provides a limit of detection (LOD) of 22 mg L−1 and a precision expressed as relative standard deviation (RSD) lower than 5%, is considerably rapid and allows for a high level of automation.

scholarly journals Analysis of the Chloroacetanilide Herbicides in Water Using SPME with CAR/PDMS and GC/ECD

2005 ◽  
Vol 88 (4) ◽  
pp. 1236-1241 ◽  
Author(s):  
Ying-Ming Hwang ◽  
Yih-Gang Wong ◽  
Wu-Hsiung Ho
Keyword(s):  
Humic Acid ◽  
Ph Value ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Standard Addition ◽  
Electron Capture Detection ◽  
Detection Analysis ◽  
Salt Addition ◽  
Chloroacetanilide Herbicides ◽  
Relative Standard

Abstract The solid-phase microextraction (SPME) technique using a 75 mm film of carboxen/polydimethylsiloxane was applied to the analysis of chloroacetanilide herbicides (acetochlor, alachlor, butachlor, metolachlor, and propachlor) residues. The feasibility of SPME with gas chromatography electron capture detection analysis has been evaluated. The effects of experimental parameters such as magnetic stirring, salt addition, humic acid addition, pH value, and extraction time, as well as desorption temperature and time, were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The inhibition of humic acid to the extraction of chloroacetanilide herbicides was observed. A standard addition method for calibration was recommended to reduce deviations caused by matrix interferences. The proposed method provided a simple and rapid analytical procedure for chloroacetanilide herbicides in water with limits of detection 0.002–0.065 μg/L for deionized water, and 0.005–0.22 μg/L for farm water. The relative standard deviations (n = 5) for analyses of farm water were 7–20% for 0.5 μg/L chloroacetanilide herbicides. This application was illustrated by the analysis of sample collected from farm water in the Chung-hwa area, Taiwan.

scholarly journals Estimating Diphenylamine in Gunshot Residues from a New Tool for Identifying both Inorganic and Organic Residues in the Same Sample

Separations ◽  
2019 ◽  
Vol 6 (1) ◽  
pp. 16 ◽  
Author(s):  
Ana Argente-García ◽  
Lusine Hakobyan ◽  
Carmen Guillem ◽  
Pilar Campíns-Falcó
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
High Sensitivity ◽  
Capillary Liquid Chromatography ◽  
Organic Residues ◽  
Cotton Swab ◽  
Gunshot Residues ◽  
Relative Standard ◽  
On Line ◽  
Inorganic And Organic

A method involving the collection and determination of organic and inorganic gunshot residues on hands using on-line in-tube solid-phase microextraction (IT-SPME) coupled to miniaturized capillary liquid chromatography with diode array detection (CapLC-DAD) and scanning electron microscopy coupled to energy dispersion X-ray (SEM-EDX), respectively, for quantifying both residues was developed. The best extraction efficiency for diphenylamine (DPA) as the main target among organic residues was achieved by using a dry cotton swab followed by vortex-assisted extraction with water, which permits preservation of inorganic residues. Factors such as the nature and length of the IT-SPME extractive phase and volume of the sample processed were investigated and optimized to achieve high sensitivity: 90 cm of TRB-35 (35% diphenyl, 65% polydimethylsiloxane) capillary column and 1.8 mL of the processed sample were selected for the IT-SPME. Satisfactory limit of detection of the method for analysis of DPA deposited on shooters’ hands (0.3 ng) and precision (intra-day relative standard deviation, 9%) were obtained. The utility of the described approach was tested by analyzing several samples of shooters’ hands. Diphenylamine was found in 81% of the samples analyzed. Inorganic gunshot residues analyzed by SEM-EDX were also studied in cotton swab and lift tape kit samplers. Optical microscopy was used to see the inorganic gunshot residues in the cotton swab samplers. The lift tape kits provided lesser sensitivity for DPA than dry cotton swabs—around fourteen times. The possibility of environmental and occupational sources could be eliminated when DPA was found together with inorganic residues. Then, the presence of inorganic and organic residues in a given sample could be used as evidence in judicial proceedings in the forensic field.

scholarly journals Solid phase selective separation and green preconcentration of Cu, Zn, Pb and Cd in drinking water by using novel functionalized resin

2009 ◽  
Vol 7 (4) ◽  
pp. 945-954 ◽  
Author(s):  
Nagwa Burham ◽  
Sami Azeem ◽  
Mohamed El-Shahat
Keyword(s):  
Drinking Water ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Exchange Capacity ◽  
Coupling Reactions ◽  
Lead And Cadmium ◽  
Sample Flow Rate ◽  
Relative Standard ◽  
Copper Zinc ◽  
Ph Range

AbstractA new solid — phase extraction sorbent was developed based on stepwise anchoring of two ligand molecules for the determination of copper, zinc, lead and cadmium in drinking water by flame AAS. Amberlite XAD-2 functionalized with 4′-(2-hydroxyphenylazo)-3′-methyl-1′-phenyl-2′-pyrazolin-5′-one (HPAPyr) was utilized for preconcentration/separation of these elements. The sorbent was prepared by two successive azo coupling reactions. First, 2-aminophenol was anchored to the amino groups in the resin resulted from nitration followed by reduction. Then, the resulted 2-aminophenol functionalized resin was further diazotized and coupled to the pyrazolone compound and the final product HPAPyr-XAD-2 was characterized by IR and elemental analysis. The optimum pH range for sorption, shaking time, exchange capacity, sample flow rate, preconcentration factor and interference from co-existing ions were investigated. All metal ions were quantitatively desorbed from the resin by 4.5 mol L−1 nitric acid solution. The sorbent provides limit of detection within the range 0.9–3.3 µg L−1 and concentration factor up to 250. The procedure was validated by analysis of certified material NIST-SRM 1577b. Application to drinking water showed satisfactory results with relative standard deviation RSD ≤ 8.5%.

scholarly journals Carbon and Tin-Based Polyacrylonitrile Hybrid Architecture Solid Phase Microextraction Fiber for the Detection and Quantification of Antibiotic Compounds in Aqueous Environmental Systems

Molecules ◽  
2019 ◽  
Vol 24 (9) ◽  
pp. 1670 ◽  
Author(s):  
Sandip Mondal ◽  
Jialing Jiang ◽  
Yin Li ◽  
Gangfeng Ouyang
Keyword(s):  
Solid Phase Microextraction ◽  
Tin Dioxide ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Tap Water ◽  
Coefficient Of Determination ◽  
Lower Amount ◽  
Custom Made ◽  
Relative Standard ◽  
Detection And Quantification

In this study, the detection and quantification of multiple classes of antibiotics in water matrices are proposed using a lab-made solid phase microextraction (SPME) fiber coupled with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lab-made fiber was prepared using a graphene oxide (G), carbon nanotubes (C), and tin dioxide (T) composite, namely GCT, with polyacrylonitrile (PAN) as supporting material. The detected antibiotics were enrofloxacin, sulfathiazole, erythromycin, and trimethoprim. The custom-made fiber was found to be superior compared with a commercial C18 fiber. The excellent reproducibility and lower intra-fiber relative standard deviations (RSDs 1.8% to 6.8%) and inter-fiber RSDs (4.5% to 8.8%) made it an ideal candidate for the detection of traces of antibiotics in real environmental samples. The proposed validated method provides a satisfactory limit of detection and good linear ranges with higher (>0.99) coefficient of determination in the aqueous system. Application of the method was made in different real water systems such as river, pond and tap water using the standard spiking method. Excellent sensitivity, reproducibility, lower amount of sample detection and higher recovery was found in a real water sample. Therefore, the extraction method was successfully applied to the detection and quantification of multiple classes of antibiotics in different aqueous systems with satisfactory results.

Determination of Oxytetracycline Residues in Matrixes from a Freshwater Recirculating Aquaculture System

2002 ◽  
Vol 85 (2) ◽  
pp. 341-348
Author(s):  
Mary C Carson ◽  
Graham Bullock ◽  
Julie Bebak-Williams
Keyword(s):  
Ethylenediaminetetraacetic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Recirculating Aquaculture System ◽  
Phase Gradient ◽  
Recirculating Aquaculture ◽  
Aquaculture System ◽  
Solid Phase Extraction Cartridge ◽  
Relative Standard ◽  
Tank Water

Abstract This paper describes related procedures to determine the amount of oxytetracycline (OTC) present in trout tissue (muscle with skin attached), biofilter sand, sediment, and tank water from a recirculating aquaculture system. OTC was extracted from the matrixes by different techniques, depending on complexity of the matrix and desired OTC detection level in that matrix. Listed in order of increasing complexity, OTC was extracted from tank water by dilution with acidic buffer containing ethylenediaminetetraacetic acid (EDTA); from biofilter sand by shaking with 0.1N HCl; from sediment by homogenization and shaking with buffer/EDTA; and from ground trout by homogenization and shaking with buffer/EDTA (twice), with further cleanup and concentration of the extract on a polymeric solid-phase extraction cartridge. The 4 procedures all used the same reversed-phase gradient chromatography on a polymeric column with UV detection at 350 nm. The lower limit of detection (estimated) and upper limit of validation for each of these 4 matrixes were 0.04–4.0 μg/g (ppm; trout), 0.03–20 ppm (biofilter sand), 1–6000 ppm (sediment), and 0.003–10 ppm (water). Recoveries ranged from 82 to 108%, with relative standard deviation &lt;20% over the applicable concentration ranges. These procedures were used to monitor OTC residues resulting from medicated feed administered to rainbow trout in a recirculating aquaculture system.

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