scholarly journals Determination of Capsaicin and Dihydrocapsaicin in Some Chilli Varieties using Accelerated Solvent Extraction Associated with Solid-Phase Extraction Methods and RP-HPLC-Fluorescence

2012 ◽  
Vol 9 (3) ◽  
pp. 1550-1561 ◽  
Author(s):  
Saksit Chanthai ◽  
Jureerat Juangsamoot ◽  
Chalerm Ruangviriyachai ◽  
Suchila Techawongstien

Reversed phase-HPLC with fluorescence detection of two major capsaicinoids was described. Isocratic elution using a ratio of methanol and deionized water (66:34, v/v) as mobile phase was used at a flow rate of 0.9 mL/min with well achieved separation within 6 min. Under optimum conditions, their analytical figures of merit for the HPLC method were validated. The linearity was in the range of 1.0-25.0 μg/mL with multiple determination coefficients of higher than 0.995. The limit of detection was ranged of 0.008-0.01 μg/mL. The repeatability and reproducibility of the retention time and peak area for these compounds were in good precision with their relative standard deviations (RSDs) lower than 1% and 5%, respectively. Both capsaicin and dihydrocapsaicin were extracted using an accelerated solvent extraction (ASE) of methanol as an extraction solvent for 5 min static time with 3 cycles. The methanolic extracts were subjected to clean up with C18solid-phase extraction (SPE) with its recoveries ranking of 90.2-98.0%. The method recoveries of real samples were found to be 60.7-98.6%. The optimized extraction method were applied for the determination of the two capsaicinoids in ten vareities of hot chilli pepper samples. Total contents of capsaicinoids were found in the range of 2,307.0-9047.3 μg/g DW with their corresponding Scoville heat unit (SHU) of 34,600-135,700. Additionally, the contents of capsaicinoids using external calibration method comparing with those of standard addition were not significantly different, indicating accuracy of the method. Mostly, the contents of capsaicin found in these real samples were rather higher than those of dihydrocapsaicin.

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi

A new solid phase extraction procedure was developed for preconcentration of iron(II) using silica gel-polyethylene glycol (silica-PEG) as an adsorbent. The method is based on retention of iron(II) as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1of sulfuric acid-acetone mixture (1:2) and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1of iron(II). The limit of detection based on3Sbwas 0.57 ng mL−1and relative standard deviations (R.S.D) for ten replicate measurements of 12 and 42 ng mL−1of iron(II) were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II) in water, multivitamin tablet, and spinach samples.


2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Haihong Li ◽  
Mingli Ye ◽  
Fangfang Wu ◽  
Xuyang Zhao ◽  
Lifeng Wang ◽  
...  

An analysis method was established to determine 14 organophosphorus ester (OPE) flame retardants in fall protection equipment by combining accelerated solvent extraction (ASE) and solid-phase extraction (SPE) with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The ASE parameters were optimized as follows: static extraction with acetonitrile at 80°C for 5 min for two cycles. The combined extract was purified with the ENVI-18 cartridge before further analysis. A HILIC column was used to separate the OPEs using an acetonitrile/water mixture as the mobile phase with the detection by the electrospray ionization mass spectrometry, which was operated under the positive mode. Under optimized conditions, the limit of detection for the target OPEs ranged in 0.015–1.33 ng/g, with a spike recovery of 71.6%–114% and a relative standard deviation of 0.8%–11.2%. The developed method was used to analyze OPEs in fall protection equipment (safety helmets and ropes), where OPEs were all detectable. Safety ropes displayed a higher concentration of OPEs than ones in safety helmets, with the pollutants being mainly triphenyl phosphate, 2-ethylhexyl diphenyl phosphate (EHDPP), tri(2-ethylhexyl) phosphate, and tri-n-butyl phosphate in the range of 11.07 ng/g‒815.53 ng/g. The EHDPP was the dominant compound in safety helmets with the concentration from 26.84 to 95.29 ng/g, while the other OPEs in safety helmets were lower than 5.136 ng/g. The potential health and environmental risks of these fall protection equipment during their use and disposal call for further attention.


2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  

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.


2018 ◽  
Vol 42 (8) ◽  
pp. 5806-5813 ◽  
Author(s):  
Rohullah Kashanaki ◽  
Homeira Ebrahimzadeh ◽  
Morteza Moradi

D-μ-SPE-SUPRAS-ME followed by GFAAS was successfully used for preconcentration and determination of copper in real samples.


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