scholarly journals Rapid Method for the Determination of Capsaicin and Dihydrocapsaicin in Gochujang Using Ultra-High-Performance Liquid Chromatography

2010 ◽  
Vol 93 (6) ◽  
pp. 1905-1911 ◽  
Author(s):  
Jaeho Ha ◽  
Hye-Young Seo ◽  
You-Shin Shim ◽  
Hyun-Jin Nam ◽  
Homoon Seog ◽  
...  

Abstract A sensitive and specific heating block method coupled with ultra-HPLC (u-HPLC) was developed for the analysis of capsaicin in Gochujang and validated by comparing with a conventional HPLC (AOAC Method 995.03). The method validation parameters yielded good results, including linearity, precision, accuracy, and recovery. The u-HPLC separation was performed on a reversed C18 column (50 2 mm id, particle size 2 m), followed by fluorescence detection (excitation 280 nm, emission 325 nm). Methanol was used as the extracting solvent, and the amount of sample taken was approximately 0.2 g; the optimum amount of extraction solvent and extraction time were 15 mL and 1 h, respectively. The recovery of capsaicin in Gochujang was more than 93, and the LOD and LOQ of the u-HPLC analysis were 0.05 and 0.16 g/g for capsaicin and 0.05 and 0.16 g/g for dihydrocapsaicin. The calibration graphs for capsaicin and dihydrocapsaicin were linear from 0.2 to 10.0 g/mL for u-HPLC. The interday and intraday precisions (RSD values) were <6.27.

2012 ◽  
Vol 95 (2) ◽  
pp. 517-522 ◽  
Author(s):  
You -Shin Shim ◽  
Ki-Jin Kim ◽  
Dongwon Seo ◽  
Masahito Ito ◽  
Hiroaki Nakagawa ◽  
...  

Abstract A rapid and novel ultra-HPLC (u-HPLC) method for the determination of vitamins A (retinol) and E (α-, γ-, and δ-tocopherol) in foods was validated in terms of its precision, accuracy, and linearity. The u-HPLC separation was performed on an RP C18 column (particle size 2 μm, id 2 mm, and length 75 mm), followed by fluorescence detection. The recovery of retinol was more than 84.58%; the LOD and LOQ of the u-HPLC analysis were 0.015 and 0.045 mg/kg, respectively. The intraday and interday precision was less than 9.12%. The recoveries of α-, γ-, and δ-tocopherol were more than 81.37%; the LOD and the LOQ were 0.014, 0.002, and 0.001 mg/kg and 0.042, 0.005, and 0.004 mg/kg, respectively. All calibration curves had good linearity (r2 = 0.99) within the test ranges. The novel, rapid method coupled to u-HPLC can provide significant improvements in the speed, sensitivity, and resolution compared with a conventional HPLC method.


2018 ◽  
Vol 69 (3) ◽  
pp. 627-631 ◽  
Author(s):  
Viorica Ohriac (Popa) ◽  
Diana Cimpoesu ◽  
Adrian Florin Spac ◽  
Paul Nedelea ◽  
Voichita Lazureanu ◽  
...  

Pain is defined as a disagreeable sensory and emotional experience related to a tissue or potential lesion. Paracetamol (Acetaminophen) is the most used non-morphine analgesic. For the determination of paracetamol we developed and validated the high performance liquid chromatography (HPLC) analysis using a Dionex Ultimate 3000 liquid chromatograph equipped with a multidimensional detector. After determining the optimum conditions of analysis (80/20 water / acetonitrile mobile phase, flow rate 1.0 mL / min, detection wavelength 245 nm) we validated the method following the following parameters: linearity of response function, linearity of results, limit (LD = 0.66 mg / mL) and quantification limit (LQ = 2.00 mg / mL), and precision. The method of determining paracetamol by HPLC was applied to 30 samples of serum collected from patients who had pain and were treated with paracetamol.


Author(s):  
Klaudia Kokoszka ◽  
Agnieszka Kobus ◽  
Sylwia Bajkacz

The residues of antimicrobials used in human and veterinary medicine are popular pollutants of anthropogenic origin. The main sources of introducing antimicrobials into the environment are sewage treatment plants and the agricultural industry. Antimicrobials in animal manure contaminate the surrounding soil as well as groundwater, and can be absorbed by plants. The presence of antimicrobials in food of plant origin may pose a threat to human health due to their high biological activity. As part of the research, a procedure was developed for the extraction and determination of ciprofloxacin, enrofloxacin, cefuroxime, nalidixic acid and metronidazole in environmental samples (soil and parsley root). An optimized solid-liquid extraction (SLE) method was used to separate antimicrobials from the solid samples and a mixture of citrate buffer (pH = 4): methanol (1:1; v/v) was used as the extraction solvent. Solid phase extraction (SPE) with OASIS® HLB cartridges was used to purify and pre-concentrate the sample. The recovery of the developed method was in the range of 55–108%. Analytes were determined by high-performance liquid chromatography coupled with an ultraviolet (UV) detector and a tandem mass spectrometer (HPLC-UV-MS/MS). The procedure was validated and applied to the determination of selected antimicrobials in soil and parsley root samples. Five types of soil and five types of parsley roots of different origins were analyzed. The presence of nalidixic acid in the parsley root samples was found in the concentration range of 0.14–0.72 ng g−1. It has been shown that antimicrobials are absorbed by the plant and can accumulate antimicrobials in its edible parts.


Amino Acids ◽  
2021 ◽  
Author(s):  
Grażyna Gałęzowska ◽  
Joanna Ratajczyk ◽  
Lidia Wolska

AbstractThe quantitation and qualification of amino acids are most commonly used in clinical and epidemiological studies, and provide an excellent way of monitoring compounds in human fluids which have not been monitored previously, to prevent some diseases. Because of this, it is not surprising that scientific interest in evaluating these compounds has resurfaced in recent years and has precipitated the development of a multitude of new analytical techniques. This review considers recent developments in HPLC analytics on the basis of publications from the last few years. It helps to update and systematize knowledge in this area. Particular attention is paid to the progress of analytical methods, pointing out the advantages and drawbacks of the various techniques used for the preparation, separation and determination of amino acids. Depending on the type of sample, the preparation conditions for HPLC analysis change. For this reason, the review has focused on three types of samples, namely urine, blood and cerebrospinal fluid. Despite time-consuming sample preparation before HPLC analysis, an additional derivatization technique should be used, depending on the detection technique used. There are proposals for columns that are specially modified for amino acid separation without derivatization, but the limit of detection of the substance is less beneficial. In view of the fact that amino acid analyses have been performed for years and new solutions may generate increased costs, it may turn out that older proposals are much more advantageous.


Food systems ◽  
2021 ◽  
Vol 4 (2) ◽  
pp. 144-153
Author(s):  
Ju. V. Nikitina ◽  
E. V. Topnikova ◽  
O. V. Lepilkina ◽  
O. G. Kashnikova

The features of technologies for low- and lactose-free dairy products, which provide for special operations to hydrolyze lactose or remove it using ultra- or nanofiltration followed by hydrolysis of the residual amount, are considered. Dairy products manufactured using these technologies in different countries as well as enterprises leading in this field of production are presented. The analysis of the methods used to determine the quantitative content of residual lactose in low- and lactose-free dairy products is carried out: enzymatic, HPLC, HPAEC-PAD, amperometric biosensors, Raman spectroscopy. Due to the dairy industry’s need for analytical methods for the determination of lactose in milk and dairy products with low- or lactose-free content, the AOAC Stakeholder Group on Strategic Food Analysis Methods approved Standard Performance Requirements for Biosensor Methods (SMPR®) 2018.009. These requirements were introduced for the quantitative determination of lactose in milk as well as in dairy and milk-containing products with a low or no lactose content. The biosensor method is recommended for use as the official first step of AOAC method. Additionally, it is advisable to use high performance liquid chromatography (HPLC) with mass spectrometric detection, as well as high performance anion exchange chromatography with pulsed amperometric detection (HPAEC-PAD) as an international standard method of analysis for the determination of lactose in milk with low- or lactose-free content.


2022 ◽  
Vol 41 (1) ◽  
pp. 34-62
Author(s):  
Andrea Dandić ◽  
Katarina Rajkovača ◽  
Marija Jozanović ◽  
Iva Pukleš ◽  
Aleksandar Széchenyi ◽  
...  

Abstract Nonsteroidal anti-inflammatory drugs (NSAIDs) are the first choice of treatment for rheumatic disorders and other degenerative inflammatory diseases. One of them, indomethacin (INDO), is highlighted in this study. With its analgesic, antipyretic, and anti-inflammatory properties, it is one of the most powerful drugs used in various clinical trials and therapies related to the mechanism of blocking prostaglandin synthesis, thus reducing and eliminating many inflammatory conditions in patients. To ensure the efficacy and safety of this drug in pharmaceutical and clinical use, precise product quality control is required. Such control is performed with routine pharmaceutical analysis using various chemical methods by which INDO is identified as a separate active ingredient in the multicomponent system of a complete pharmaceutical form. In addition, the determination of INDO is important in clinical practice, where its concentration is determined in different biological samples, ensuring better monitoring of a particular therapy. The most commonly used methods for the determination of INDO are high-performance liquid chromatography (37% of developed methods), voltammetry (16% of developed methods), and UV spectroscopy (11% of developed methods). However, each of these methods must provide precise validation parameters. A combination of analytical methods can lead to more precise results and safer application in practice.


2021 ◽  
Vol 16 ◽  
pp. 1-9
Author(s):  
Muhammad Abdurrahman Munir ◽  
Muhammad Mukram Mohamed Mackeen ◽  
Lee Yook Heng ◽  
Khairiah Haji Badri

Histamine is a heterocyclic amine shaped by decarboxylation of the histidine. It is a compound that lack chromophore and involatile. However, the detection of histamine is imperative due to the characteristic of histamine has given several disadvantages in food industry. This paper describes methods for histamine detection by employing high performance liquid chromatography and gas chromatography. The derivatization techniques required for both methods in order to increase the sensitivity of chromatography analysis. Two derivatizing agents were applied in this study such as 9-flourenilmethyl chloroformate (FMOC – Cl) for HPLC analysis whereas for GC analysis a N,O-bis (trimethylsilyl)acetamide (BSA) was used. Method validation was in accordance to Commission Decision 657/2002/CE. The validation of specificity, linearity, precision, accuracy, detection limit and quantitation limit results indicate that the methods were acceptable. The linear range for both methods were at 0.16 – 5.00 µg∙mL-1. The determination of histamine using GC showed the superiority of this instrument compared to HPLC. Method applicability was also checked on real sample namely mackerel in order to acquire a satisfactory recovery for both methods.


2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.


2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.


2015 ◽  
Vol 768 ◽  
pp. 15-24
Author(s):  
Pu Wang ◽  
Hui Ling Liu ◽  
Bing Wang ◽  
Xiu Wen Cheng ◽  
Qing Hua Chen ◽  
...  

In this study, a rapid and selective method has been developed to determine PENG residues in waste penicillium chrysogenum by using SPE cleanup strategy followed by HPLC. Furthermore, some parameters which influenced the extraction efficiency including extraction mode, solvent and time, while washing solution and eluting solution for SPE were systematically investigated. It should be noted that the extraction process was carried out in a single step by mixing the extraction solvent acetonitrile: formic acid in aqueous solution and chrysogenum samples under ultrasound. The SPE procedure was conducted using Oasis HLB as the clean up cartridge, n-hexane as washing solution, and mixture of acetonitrile and methanol as eluting solution. Under the optimized conditions, the linear of PENG are in the range of 0.1-2000 μg/mL, with the correlation was R2>0.99. In addition, the recoveries of PENG in these samples at three fortification levels of 800-1800mg/kg were 74.98% to 113.47% are obtained, respectively. Moreover, a limits of detection (0.006 mg/kg) and quantification (0.02 mg/kg) could be achieved.


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