scholarly journals Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil

Molecules ◽  
2020 ◽  
Vol 25 (6) ◽  
pp. 1415
Author(s):  
Rui Song ◽  
Qincheng Chen ◽  
Lili Yan ◽  
Pinhua Rao ◽  
Peng Sun ◽  
...  
Keyword(s):  
Response Surface ◽  
High Performance ◽  
Detection Method ◽  
Simultaneous Detection ◽  
Animal Husbandry ◽  
Ultrasound Assisted Extraction ◽  
Buffer Solution ◽  
Solution Ph ◽  
Simultaneous Extraction ◽  
17Β Estradiol

Antibiotics and hormones widely exist in fertilizers and manures, which are excessively used in agriculture and animal husbandry. Considering their potential harm to the environment and human health, the detection of antibiotics and hormones has become a necessity. However, current methods find it difficult to simultaneously extract and detect antibiotics and hormones in soil and to maintain a high level of accuracy and a low cost. In this study, a straightforward, convenient, and simultaneous extraction and detection method of a representative antibiotic (sulfamethoxazole, SMZ) and hormone (17β-Estradiol, E2) in soil has been established. Ultrasound-assisted extraction (UAE) was used in the pretreatment process and high-performance liquid chromatography with the ultraviolet detector (HPLC-UV) method was then chosen in the detection process. By means of single factors and response surface experiments, optimal extraction conditions were a 41-mL buffer solution (pH 4.27) mixed with 1 g of soil sample, an ultrasonication time of 36 min, an ultrasonication temperature of 25 °C, and two extraction cycles. The detection limits of 0.3–10 μg/kg and quantification limits of 1–30 μg/kg have been obtained. Finally, the optimized simultaneous extraction and detection method was validated by three different real soil samples with recoveries ranging from 79.49% to 86.47%.

OPTIMISATION AND VALIDATION OF HPLC METHOD FOR SIMULTANEOUS QUANTIFICATION OF RIFAMPICIN, ISONIAZID, PYRAZINAMIDE, AND ETHAMBUTOL HYDROCHLORIDE IN ANTI-TUBERCULOSIS 4-FDC TABLET

2015 ◽  
Vol 77 (1) ◽  
Author(s):  
Sholihul Khoiri ◽  
Sudibyo Martono ◽  
Abdul Rohman
Keyword(s):  
High Performance ◽  
Phosphate Buffer Solution ◽  
Gradient Elution ◽  
Hplc Method ◽  
Fixed Dose ◽  
Buffer Solution ◽  
Solution Ph ◽  
Combination Tablet ◽  
Simultaneous Quantification ◽  
Dose Combination

High-performance liquid chromatography (HPLC) method has been developed and validated for the simultaneous quantification of four components, namely rifampicin (RIF), isoniazid (INH), pyrazinamide (PYR), and ethambutol hydrochloride (ETM), contained in anti-tuberculosis drugs in fixed dose combination tablet (4-FDC). In order to increase the sensitivity of EMB, the pre-column derivatization technique with phenethyl isocyanate (PEIC) was carried out. The separation was accomplished using Waters Symmetry C8 (250× 4.6 mm i.d.; 5 μm) at 30oC. The mobile phase used was a mixture of acetonitrile and 20 mM phosphate buffer solution (pH 6.8) containing triethylamine and delivered at 1.5 mL/minute using gradient elution. TheUV detector was set at 210 nm. The method was validated in terms of selectivity, linearity, accuracy, precision, detection limit, quantification limit, and robustness according to International Conference on Harmanization (ICH). The optimized method is succcesfully used for quantitative analysis of RIF, INH, PYR and ETM in 4-FDC tablets. The level of these drugs in 4-FDC tablets were in accordance to that specified in Indonesian pharmacopeia.

scholarly journals Fluorescence-Based On-Resin Detection of Three Model Proteases

Chemosensors ◽  
2021 ◽  
Vol 9 (12) ◽  
pp. 359
Author(s):  
David Milićević ◽  
Jan Hlaváč
Keyword(s):  
Fluorescent Dyes ◽  
Simultaneous Detection ◽  
Solid Support ◽  
Buffer Solution ◽  
Solution Ph ◽  
New Approach ◽  
Backbone Amide ◽  
Cleavable Peptide ◽  
Backbone Amide Linker ◽  
Competitive Activities

A new approach to on-resin detection of three model proteases (trypsin, chymotrypsin, and thrombin) has been developed, while at the same time already described methodology for simultaneous detection of two enzymes (trypsin and chymotrypsin) has been additionally generalized. Appropriate immobilized substrates, comprising specifically cleavable peptide sequences capped with fluorescent dyes, have been synthesized on Rink Amide PEGA resin or Amino PEGA resin modified with backbone amide linker (BAL). Resulting solid support-bound probes were then dispersed into Tris-HCl buffer solution (pH = 8.0) and subjected to enzymatic cleavage. Liberated fluorophores have been tracked by fluorescence measuring. The competitive activities of studied proteases towards the thrombin probe have been efficiently limited and controlled by employing a Bowman-Birk inhibitor into a system.

scholarly journals Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure

2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Lanqing Li ◽  
Mingxing Sun ◽  
Hui Zhou ◽  
Yun Zhou ◽  
Ping Chen ◽  
...  
Keyword(s):  
Response Surface ◽  
Extraction Method ◽  
Extraction Procedure ◽  
Extraction Time ◽  
Extraction Temperature ◽  
Ultrasound Assisted Extraction ◽  
Solution Ph ◽  
Assisted Extraction ◽  
Ultrasound Assisted

A rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influence of several variables on the efficiency of the extraction procedure was investigated by single-factor experiments. The temperature, pH, and amount of extraction solution were selected for optimization experiment using response surface methodology. The calibration curves showed good linearity (R2>0.99) for all analytes in the range of 0.1–20 μg/mL. The four antibiotics were successfully extracted from manure with recoveries ranging from 81.89 to 92.42% and good reproducibility (RSD, <4.06%) under optimal conditions, which include 50 mL of McIlvaine buffer extraction solution (pH 7.15) mixed with 1 g of manure sample, extraction temperature of 40°C, extraction time of 10 min, and three extraction cycles. Method quantification limits of 1.75–2.32 mg/kg were obtained for the studied compounds. The proposed procedure demonstrated clear reductions in extraction time and elimination of cleanup steps. Finally, the applicability to tetracyclines antibiotics determination in real samples was evaluated through the successful determination of four target analytes in swine, cow manure, and mixture of animal manure with inorganic fertilizer.

scholarly journals Simultaneous quantifications of four purine derivatives biomarkers in cow milk by SPE HPLC-DAD

2021 ◽  
Vol 39 (No. 2) ◽  
pp. 122-130
Author(s):  
Mihaela Vlassa ◽  
Miuta FILIP ◽  
Catalin DRAGOMIR
Keyword(s):  
Uric Acid ◽  
High Performance ◽  
Solid Phase ◽  
Cow Milk ◽  
Good Precision ◽  
Purine Derivatives ◽  
Buffer Solution ◽  
Solution Ph ◽  
Relative Standard ◽  
Array Detection

In this study, simultaneous quantification of allantoin, uric acid, xanthine, and hypoxanthine in cow milk by solid phase extraction (SPE) and high performance liquid chromatography-diode array detection (HPLC-DAD) method was perform. Five different SPE cartridges were tested in order to evaluate the isolation of purine derivatives (PD) from cow milk. Chromatography was carried out on ODS-2 Hypersil column and 0.05 M (NH<sub>4</sub>)<sub>2</sub>HPO<sub>4</sub> buffer solution (pH = 7.76) as mobile phase. The HPLC-DAD validated method showed a linearity with regression coefficients higher than 0.999 and the limits of detection and quantification with values in the range 0.09–0.74 µg mL<sup>–1</sup> and 0.27–2.24 µg mL<sup>–1</sup>, respectively. The method showed good precision with a relative standard deviation (RSD) below 4.48%, while the accuracy ranged from 95.34 to 104.47% for all analytes. The best recovery degree of PD by SPE were obtained on Strata SCX cartridge for xanthine (87.79%) and hypoxanthine (89.02%); on Strata NH<sub>2</sub> for allantoin (35.09%) and on Strata C8 for uric acid (101.08%). Finally, the HPLC-DAD method with SPE on SCX cartridges was applied to quantify the PD in a batch of thirty cow milk samples.

scholarly journals THE INFLUENCE OF FERMENTATION AND LONG STORAGE ON THE SILAGE OF CORN TEBON

2016 ◽  
Vol 1 (2) ◽  
pp. 47-54
Author(s):  
La Agus
Keyword(s):  
Animal Husbandry ◽  
Nutrient Content ◽  
Corn Silage ◽  
Buffer Solution ◽  
Solution Ph ◽  
Fermentation Time ◽  
Randomized Design ◽  
Before And After ◽  
Materials Used ◽  
Long Storage

The study aims to determine the effect of fermentation time complete feed and silage of Tebon corn to changes in pH and nutrient content. This research was conducted in January to March 2015, in the Laboratory airy College of Agricultural Sciences (STIPER) Kendari and analysis of feed materials to be carried out at the Laboratory of Animal Nutrition and Feed Faculty of Animal Husbandry Haluoleo university. Materials used in this study were aged 60-70 days corn Tebon, pollard 20%; copra 20%; premix 30%; corn Empok 25%; salt 2.5%; minerals 2.5%, Aquadest, a buffer solution pH 7. The catalyst, concentrated H2SO4, distilled water, 0,1N H2SO4, NaOH 40%, indicatormix, 0,1N NaOH. Equipment used in this study include: chopper, plastic, rope scales, vacuum, freezer, Erlenmeyer, pH meter, analytical balance, pumpkin Kjeldhal, Erlenmeyer, glass beaker, destructor, distillation, titration tools, ovens and furnaces. The method used in this study is completely randomized design experiment Nested with 2 treatments, three long storage and 3 replicates (2x3x3) on each treatment. The treatment tested was: Concentrate + Tebon corn with different fermentation time, concentrate + corn silage Tebon with different fermentation time, then do Silage-making, mixing Silage, Silage Testing. The parameters in this study the degree of acidity (pH), nutrient content includes dry matter (DM), organic matter (OM) and crude protein (CP) before and after fermentation. Based on the results of complete feed nutrient content analysis showed that each - each fermentation time treatment effect (P<0,01) to change the content of DM, OM and CP when compared to the control with the average low enough pH ranged from 4.18 to 4, 38. Based on this research can be concluded that the fermentation time very real impact on the quality of corn silage Tebon. Fermentation feed concentrate and corn Tebon (KT) decreased nutrient content higher than the complete feed made from concentrates and corn Tebon silage (KS)

scholarly journals Quantitation of Pregabalin by HPLC-UV Method using Ninhydrin Derivatization: Development and Validation

2020 ◽  
Vol 17 (1) ◽  
pp. 165-171
Author(s):  
Fathiy Mutalabisin ◽  
Abul Bashar Mohammed Helaluddin ◽  
Pinaki Sengupta ◽  
Farahidah Mohamed ◽  
Bappaditya Chatterjee
Keyword(s):  
High Performance ◽  
Phosphate Buffer Solution ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Uv Detector ◽  
Buffer Solution ◽  
Solution Ph ◽  
Acid Analogue ◽  
Development And Validation ◽  
Liquid Chromatographic

Introduction: A simple and reliable high performance liquid chromatographic method has been developed for the quantitative determination of pregabalin in bulk and dosage form. Pregabalin, a γ amino butyric acid analogue, has negligible sensitivity to UV or fluorescence detection. Hence, it has been derivatized by ninhydrin to form a chromophoric complex that could be quantified by UV detection. Materials and Methods: The concentration of ninhydrin was set to 5 mg/ml and a phosphate buffer solution (pH 7.4) was used as a solvent for the reaction. The resultant complex was separated by HPLC and detected by a UV detector at 569nm wavelength. Results: The developed method showed a linear response within 50 to 600 μg/mL of pregabalin. The method was accurate with mean recovery values within 100 ± 2%. The repeatability of the method was established by intra-day and inter-day precision study. Finally, a commercial pregabalin capsule was assayed by the developed HPLC method including ninhydrin derivatization. The result of the mean assay was found to be 100.37 ±2.94 %. Conclusion: This is the first time we are reporting pregabalin analysis using ninhydrin derivatization for HPLC analysis. Therefore, the developed method can be considered as a significant improvement in pregabalin quantitation and it can be easily applied for routine quality control tests of pregabalin.

Applications of Reversed-Phase High-Performance Liquid Chromatoraphy in Strains Identification of the Bean Sprout

2011 ◽  
Vol 347-353 ◽  
pp. 354-359
Author(s):  
Yong Zuo ◽  
Shuai Ju ◽  
Yang Li ◽  
Hui Xie ◽  
Li Ping Liu ◽  
...  
Keyword(s):  
Lactic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Phosphate Buffer Solution ◽  
Reversed Phase ◽  
Qualitative And Quantitative Analysis ◽  
Buffer Solution ◽  
Solution Ph ◽  
Bean Sprout ◽  
Qualitative And Quantitative

Lactic acid which was fermented by bean sprout was determined and the lactobacillus in bean sprout was identified by High-performance Liquid Chromatoraphy(HPLC). The optimal HPLC chromatographic conditions were determined as follows:Agilent XDB-C18 chromatography column with UV detection at 210nm.The mobile phase was Phosphate buffer solution（pH=2.3）:methanol:acetonitrile（95%:2%:3%）.The flow rate was 0.5ml/min.This method is accurate,Speedily and reproducible. This method can identify the lactobacillus, and gives a qualitative and quantitative analysis of the lactic acid which was the metabolites of Yibin bean sprout.

Simultaneous Detection of Three Phosphodiesterase Type 5 Inhibitors and Eight of Their Analogs in Lifestyle Products and Screening for Adulterants by High-Performance Thin-Layer Chromatography

2015 ◽  
Vol 98 (5) ◽  
pp. 1226-1233 ◽  
Author(s):  
Tiên T K Do ◽  
Grigorios Theocharis ◽  
Eike Reich
Keyword(s):  
High Performance ◽  
Simultaneous Detection ◽  
Uv Spectra ◽  
Spectrometric Analysis ◽  
Ultrasound Assisted Extraction ◽  
Phosphodiesterase Type 5 Inhibitors ◽  
Additional Degree ◽  
Preliminary Identification ◽  
Rf Values ◽  
Phosphodiesterase Type

Abstract An HPTLC method is proposed to permit effective screening for the presence of three phosphodiesterase type 5 inhibitors (PDE5-Is; sildenafil, vardenafil, and tadalafil) and eight of their analogs (hydroxyacetildenafil, homosildenafil, thiohomosildenafil, acetildenafil, acetaminotadalafil, propoxyphenyl hydroxyhomosildenafil, hydroxyhomosildenafil, and hydroxythiohomosildenafil) in finished products, including tablets, capsules, chocolate, instant coffee, syrup, and chewing gum. For all the finished products, the same simple sample preparation may be applied: ultrasound-assisted extraction in 10 mL methanol for 30 min followed by centrifugation. The Rf values of individual HPTLC bands afford preliminary identification of potential PDE5-Is. Scanning densitometry capabilities enable comparison of the unknown UV spectra with those of known standard compounds and allow further structural insight. Mass spectrometric analysis of the material derived from individual zones supplies an additional degree of confidence. Significantly, the proposed screening technique allows focus on the already known PDE5 Is and provides a platform for isolation and chemical categorization of the newly-synthesized analogs. Furthermore, the scope could be expanded to other therapeutic categories (e.g., analgesics, antidiabetics, and anorexiants) that are occasionally coadulterated along with the PDE5-Is. The method was successfully applied to screening of 45 commercial lifestyle products. Of those, 31 products tested positive for at least one illegal component (sildenafil, tadalafil, propoxyphenyl hydroxyhomosildenafil, or dimethylsildenafil).

scholarly journals Optimization of Ultrasound Assisted Extraction (UAE) of Kinsenoside Compound from Anoectochilus roxburghii (Wall.) Lindl by Response Surface Methodology (RSM)

Molecules ◽  
2020 ◽  
Vol 25 (1) ◽  
pp. 193 ◽  
Author(s):  
Biyun Yang ◽  
Mengyuan Zhang ◽  
Haiyong Weng ◽  
Yong Xu ◽  
Lihui Zeng
Keyword(s):  
Response Surface ◽  
High Performance ◽  
Dry Weight ◽  
Methanol Concentration ◽  
Ultrasonic Power ◽  
Ultrasound Assisted Extraction ◽  
Solid Ratio ◽  
Assisted Extraction ◽  
Anoectochilus Roxburghii ◽  
Ultrasound Assisted

The purpose of this study was to establish an extraction method for the kinsenoside compound from the whole plant Anoectochilus roxburghii. Ultrasound assisted extraction (UAE) and Ultra-high performance liquid chromatography (UPLC) method were used to extract and determine the content of kinsenoside, while response surface method (RSM) was used to optimize the extraction process. The best possible range for methanol concentration (0–100%), the liquid-solid ratio (5:1–30:1 mL/g), ultrasonic power (240–540 W), duration of ultrasound (10–50 min), ultrasonic temperature (10–60 °C), and the number of extractions (1–4) were obtained according to the single factor experiments. Then, using the Box-Behnken design (BBD) of response surface analysis, the optimum extraction conditions were obtained with 16.33% methanol concentration, the liquid-solid ratio of 10.83:1 mL/g and 35.00 °C ultrasonic temperature. Under these conditions, kinsenoside extraction yield reached 32.24% dry weight. The best conditions were applied to determine the kinsenoside content in seven different cultivation ages in Anoectochilus roxburghii.

Determination of Synephrine and Naringenin in Aifunuangong Pills by High Performance Capillary Electrophoresis

2013 ◽  
Vol 850-851 ◽  
pp. 1160-1163
Author(s):  
Hai Xing Liu ◽  
Qing Liu ◽  
Yi Min Feng ◽  
Lin Tong Wang ◽  
Yan Fu Huan ◽  
...  
Keyword(s):  
Capillary Electrophoresis ◽  
High Performance ◽  
Buffer Solution ◽  
Solution Ph ◽  
New Approach ◽  
Capillary Electrophoresis Method ◽  
Electrophoresis Method ◽  
High Performance Capillary Electrophoresis ◽  
Separation Of Components

This paper established high performance capillary electrophoresis method to determine synephrine and naringenin in aifunuangong pills. In 30mmol/L Na2B4O7 buffer solution (pH=10.00), effective separation of components to be tested was achieved, which provided a new approach of quality control of Chinese medicine aifunuangong pills.

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