scholarly journals Determination and validation of Tetracycline residues in Poultry by High Performance Liquid Chromatography - Diode Array Detector Technique

2019 ◽  
Vol 30 (3) ◽  
pp. 38
Author(s):  
Lobaina M Alrhia ◽  
Issam Mohamad ◽  
Sameer Mearouf

The aim of this research is separation and determination of trace Tetracycline residues in Poultry chest, thigh and liver using High Performance Liquid Chromatography - Diode Array Detector (HPLC-DAD), with a mobile phase mixture consisting of acetonitrile: methanol: oxalic acid (0.01M) (25:15:60) and chromatographic column C8. The study was done on 32 live poultry individuals. All individuals were injected in the chest by 1m of Tetracycline standard solutions, then slaughter for analysis throughout four successive days. The injection with 10×103 ppb of Tetracycline showed that the traces of Tetracycline residues (according to the Codex Alimentarius Commission) exceeded the value of the maximum residue limit (MRL = 200 ppb) in the thigh and chest meat at the 1st day and the 1st & 2nd days of slay respectively, and exceeded the value of (MRL = 600 ppb) in the liver at the 3rd and 4th days of slay. limit of detection was LOD = 0.451 ppb, limit of quantification LOQ = 1.502 ppb, and recovery percentages of Tetracycline at a concentration of 200.0 ppb for 20 sample Rec.% = (88.966 - 91.055%), (84.623 - 87.667%), (82.198 - 83.688%) for Poultry chest, thigh and liver respectively with a percentage relative standard deviations (RSD%) of < 1 %.

Author(s):  
Agna Heliade Oliveira ◽  
Valmir Gomesde Souza ◽  
FÁbio Santosde Souza ◽  
Rui Oliveira Macedo

Objective: This study aims to develop the extraction of the marker kaempferol in the fluid extract (FE) and validate an analytical method that monitors the quality of extracts of P. pyramidalis. Methods: The P. pyramidalis leaves were collected and then were dried to milling process. The extracts were drawn up at 20% weight: Volume (w/v) by maceration, and the extraction system used was hydroethanol solution ratio at 50:50 volume: Volume (v: v). From the hydroalcoholic extract, a method of extracting the kaempferol biomarker was developed and validated by high-performance liquid chromatography coupled with diode array detector. To validate a method, the following parameters were evaluated: Specificity, selectivity, linearity, limit of quantification (LOQ) and detection (LOD), precision, accuracy, robustness, and stability. Results: The method developed proved to be efficient, as it allowed the analysis of the interferents free marker, with recovery above 90%, linear over the range 1.4–26.6 μg/mL, correlation coefficient R2=0.999, and LOD and LOQ 0.07 and 0.22 μg/mL, respectively, specificity, precision, accuracy, and robustness. Conclusion: The extraction methodology of the kaempferol marker was successfully developed interferents free and the validated method by HPLC-DAD represents a useful tool in the quality control of P. pyramidalis herbal medicines.


2007 ◽  
Vol 70 (7) ◽  
pp. 1735-1738 ◽  
Author(s):  
DİREN BEYOĞLU ◽  
GÜLDEN Z. OMURTAG

This study is the first report on an investigation of the naphthalene concentration in samples of contaminated honey consumed in Turkey. Naphthalene was detected using high-performance liquid chromatography with a diode array detector at 220 nm. In one suspected contaminated specimen, the presence of naphthalene was confirmed by gas chromatography with mass spectrometry (GC-MS) at a concentration of 1.13 μg/kg. The limit of detection was 0.023 μg/g and the limit of quantification was 0.078 μg/g with signal-to-noise ratios of 3 and 10, respectively. A total of 100 samples of commercially available honey obtained from markets (53 samples) and street bazaars (47 samples) were analyzed. Mean naphthalene recovery from honey known to be contaminated with 1 μg/g was 80.4% (SD = 4.84%, n = 7).


2013 ◽  
Vol 694-697 ◽  
pp. 1047-1050
Author(s):  
Hong Jun Wang ◽  
Tie Zhong Zhou ◽  
Hong Jiang ◽  
Dan Yao ◽  
Tie Liang Wang ◽  
...  

Bangduling (BDL) oral liquid, which is a new research and development herbal preparation, comprises four traditional Chinese medicines (TCM): Radix Scutellariae, Cortex Phellodendri Chinensis, Folium Isatidis, and Radix et Rhizoma Rhei. A simple, reliable and reproducible method, based on a high performance liquid chromatography-diode array detector (HPLC-DAD) method, for establishing fingerprint of complex herbal medicine BDL oral liquid was described firstly. In order to develop and validate this HPLC-DAD method, Kromasil C18 column (S-5μm, 4.6 mm × 250 mm) was used with gradient mobile phase at the column temperature of 30°C. The mobile phase was consisted of methanol and water containing 0.1% phosphoric acid. UV wavelength was set at 254 nm. Ten batches of BDL preparations were used to establish the HPLC fingerprint. In addition, the contents of baicalin in the preparations were also determined. Validation of the analytic method was evaluated by stability, precision and repeatability test. Calibration curve for baicalin showed good linearity with R2 = 0.9992. The relative standard deviations (RSDs) value of the relative retention time and peak area in the stability, precision and repeatability test, were less than 1% and 5%, respectively. The similarity of 10 batches of BDL oral liquid was more than 0.958, which showed the preparations from different batch productions were consistent. This established determination method could be efficient to the quality control of BDL oral liquid.


2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Thiyagarajan Sathishkumar ◽  
Ramakrishnan Baskar ◽  
Mohan Aravind ◽  
Suryanarayanan Tilak ◽  
Sri Deepthi ◽  
...  

Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2±0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method.


Author(s):  
Kanan G Gamit ◽  
Niraj Y Vyas ◽  
Nishit D Patel ◽  
Manan A Raval

Objective: A study was aimed to estimate guggulsterone-Z (GZ) in Gokshuradi Guggulu (GG).Methods: An analytical method was developed and validated using Waters Alliance high-performance liquid chromatography system (Empower software), equipped with photodiode array detector. Separation was achieved using Phenomenex, C-18 (250 mm×4.6 mm, 5 μ) column. Mobile phase consisted of acetonitrile:water (70:30,v/v). Flow rate was set to 1 ml/min and detection was performed at 251 nm.Results and Discussion: Validation parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, and robustness were performed. Amount of GZ was estimated using linearity equation.Conclusion: GG was found to contain 0.815±0.03 g% w/w GZ. Validated method may be used as one of the parameters to standardize the formulation.


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