scholarly journals Residue of ochratoxin A in swine tissues: Risk assessment

2009 ◽  
Vol 17 (3-4) ◽  
pp. 56-60 ◽  
Author(s):  
Dragan Milicevic ◽  
Verica Juric ◽  
Dubravka Vukovic ◽  
Miodrag Mandic ◽  
Tatjana Baltic
Keyword(s):  
Risk Assessment ◽  
Ochratoxin A ◽  
Strong Correlation ◽  
High Performance ◽  
Plasma Samples ◽  
Pork Products ◽  
Significant Difference ◽  
Liver And Kidney ◽  
Slaughtered Pigs

Background: Samples of blood, kidney, and liver per animal were randomly selected from slaughtered pigs (n=60) and analyzed for ochratoxin A. Methods: Determination of ochratoxin A concentration in samples of kidney and liver was performed by high-performance thinlayer chromatography after immunoaffnity column clean up, while for plasma samples, a spectrofluorometric procedure was used. Results: Of the 60 plasma samples, 60% contained ochratoxin A in the range of 2.5-33.3 ng/mL (mean 3.05?5.0 ng/mL), while the incidence of ochratoxin A in kidneys and liver were very similar (70% and 65%). The average ochratoxin A concentration in liver was 3.2?4.35 ng/g (1.2-19.5 ng/g) and in kidneys was 3.97?4.47 ng/g (1.3-22.0 ng/g). A statistically significant difference (p<0.01) was found between region Backa Topola and Kovilj for both liver and kidney samples. In kidney samples originating from region Kovilj and Senta, a statistically significant difference (p<0.01) was found. Mean distribution followed the pattern: kidney>liver>serum (100>80.8>77%). The results from this survey indicated that there was a strong correlation between the ochratoxin A level in serum and liver as well as in the ochratoxin A serum in kidney (r=0.884 and r=0.896, respectively) while the strongest correlation was found between the ochratoxin A level in liver and in kidney (r=0.970). Conclusion: The results of present study show that pork tissues as well as pork products are considered an important source of ochratoxin A in humans.

Development of an HPLC-UV Method for Quantification of Stattic

2019 ◽  
Vol 15 (6) ◽  
pp. 568-573
Author(s):  
Soheil Sedaghat ◽  
Ommoleila Molavi ◽  
Akram Faridi ◽  
Ali Shayanfar ◽  
Mohammad Reza Rashidi
Keyword(s):  
High Performance ◽  
Accurate Method ◽  
Plasma Samples ◽  
Promising Target ◽  
Relative Standard ◽  
Dimerization Inhibitor ◽  
Oncogenic Protein ◽  
First Time ◽  
Transcription 3

Background: Signal transducer and activator of transcription 3 (STAT3), an oncogenic protein found constitutively active in many types of human malignancies, is considered to be a promising target for cancer therapy. Objective: In this study for the first time, a simple and accurate method has been developed for the determination of a STAT3 dimerization inhibitor called stattic in aqueous and plasma samples. Methods: A reverse-phase high-performance liquid chromatography (RP-HPLC) composed of C18 column as stationary phase, and the mixture of acetonitrile (60%) and water (40%) as mobile phase with a UV detection at 215 nm were applied for quantification of stattic. The developed method was validated by Food and Drug Administration (FDA) guideline. Results: The method provided a linear range between 1-40 and 2.5-40 µg mL-1 for aqueous and plasma samples, respectively, with a correlation coefficient of 0.999. The accuracy (as recovery) of the developed method was found to be between 95-105% for aqueous medium and 85-115% for plasma samples. The precision (as relative standard deviation) for aqueous and plasma samples was less than 6% and 15%, respectively. The sensitivity of the developed method based on FDA guideline was 1 µg mL-1 for aqueous and 2.5 µg mL-1 for plasma samples. Conclusion: These results show that the established method is a fast and accurate quantification for stattic in aqueous and plasma samples.

Solvent bar microextraction combined with HPLC-DAD for simultaneous determination of diuretics in human urine and plasma samples

2021 ◽  
Vol 22 ◽  
Author(s):  
Nabil N. AL-Hashimi ◽  
Amjad H. El-Sheikh ◽  
Manal I. Alruwad ◽  
Mohanad M. Odeh
Keyword(s):  
Simultaneous Determination ◽  
Human Urine ◽  
High Performance ◽  
Plasma Samples ◽  
Satisfactory Precision ◽  
Array Detection ◽  
Spiked Human Urine ◽  
Analytical Technology ◽  
Solvent Bar Microextraction

Background: A simple and powerful microextraction procedure, the solvent bar microextraction (SBME), was used for the simultaneous determination of two diuretics, furosemide and spironolactone in human urine and plasma samples, using high-performance liquid chromatography coupled with diode array detection (HPLC-DAD). Methods: The appropriate amount (2 µL) of 1-octanol as an organic solvent confined within (2.5 cm) of a porous hollow fiber micro-tube, sealed at both ends was used for this procedure. The conditions for the SBME were optimized in water and the analytical performance were examined in spiked human urine and plasma samples. Results: The optimized method exhibited good linearity (R2 > 0.997) over the studied range of higher than 33 to 104 µg L-1 for furosemide and spironolactone in urine and plasma samples, illustrating a satisfactory precision level with RSD values between 2.1% and 9.1%. Discussion: The values of the limits of detection were found to be in the range of 6.39 to 9.67 µg L-1, and extraction recovery˃ 58.8% for both diuretics in urine and plasma samples. The applicability and effectiveness of the proposed method for the determination of furosemide and spironolactone in patient urine samples were tested. Conclusion: In comparison with reference methods, the attained results demonstrated that SBME combined with HPLC-DAD was proved to be simple, inexpensive, and promising analytical technology for the simultaneous determination of furosemide and spironolactone in urine and plasma samples.

PSX-A-27 Late-Breaking: The sulfatase mediated regeneration of androstenone from androstenone sulfate in boar fat

2021 ◽  
Vol 99 (Supplement_3) ◽  
pp. 376-376
Author(s):  
Christine Bone ◽  
E James Squires
Keyword(s):  
Leydig Cells ◽  
High Performance ◽  
Boar Taint ◽  
Pork Products ◽  
Significant Difference ◽  
Sulfatase Activity ◽  
Steroid Sulfate ◽  
Student’S T ◽  
Entire Male ◽  
Student’S T Test

Abstract Boar taint is an off-odour or off-flavour that develops in heated pork products from entire male pigs, which is caused by the accumulation of androstenone, a sex pheromone, in the fat. However, we have previously demonstrated that a significant amount of androstenone undergoes sulfoconjugation upon synthesis in the Leydig cells and circulates in the plasma primarily as a polar steroid sulfate. Therefore, the purpose of this study was to determine if androstenone sulfate can be deconjugated within the adipose tissue by the sulfatase enzyme to return free androstenone and indirectly contribute to the development of boar taint. Backfat was obtained from 6-month-old terminal cross [Duroc x (Landrace x Yorkshire)] boars that had high (n=4) or low (n=4) sulfatase expression as determined by RT-PCR. Sulfatase activity in the fat was measured by quantifying the conversion of androstenone sulfate to free androstenone. Backfat was homogenized and the supernatant was incubated with [3H]-androstenone sulfate for 24-hours. Androstenone was extracted from the incubation using ether and steroid conversion was quantified using high-performance liquid chromatography (HPLC). Additionally, fat androstenone concentrations were quantified using an established HPLC procedure. Statistical analysis was conducted using a Student’s t-test. There was a significant difference (p=0.04) in the expression of sulfatase between the high (2.99 ± 0.67) and low (1.21 ± 0.19) sulfatase boars and the percentage of androstenone sulfate that was converted to free androstenone was proportional to the expression of sulfatase. Interestingly, the expression of sulfatase was positively related to the concentration of androstenone in the fat in boars with high sulfatase expression; however, this relation was not as strong in animals with low sulfatase expression. These preliminary results suggest that the development of boar taint may occur indirectly through the deconjugation of androstenone sulfate in boars with high expression of sulfatase in the fat.

HPTLC Separation of a Hepatoprotective Combination in Pharmaceutical Formulation and Human Plasma

2020 ◽  
Vol 58 (5) ◽  
pp. 411-417
Author(s):  
Maimana A Magdy ◽  
Rehab M Abdelfatah
Keyword(s):  
Human Plasma ◽  
High Performance ◽  
Limit Of Detection ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Spiked Plasma ◽  
Significant Difference ◽  
Developing System

Abstract A binary mixture of Silymarin (SR) and Vitamin E (VE) acetate, of an antioxidant and a hepatoprotective effect, has been analyzed using a sensitive, selective and economic high performance thin layer chromatographic (HPTLC) method in their pure forms, pharmaceutical formulation and spiked human plasma. SR and VE were separated on 60F254 silica gel plates using hexane:acetone:formic acid (7:3:0.15, v/v/v) as a developing system with UV detection at 215 nm. The method was evaluated for linearity, accuracy, precision, selectivity, limit of detection (LOD) and limit of quantification (LOQ). SR and VE were detected in the linear range of 0.2–2.5 and 0.2–4.5 μg/band, respectively. Method validation was done as per ICH guidelines and acceptable results of accuracy of 99.86 ± 1.190 and 100.22 ± 1.609 for SR and VE, respectively were obtained. The method has been successfully applied for determination of the studied drugs in their pharmaceutical formulation without any interference from excipients, and in spiked plasma samples. Results obtained by the developed HPTLC-densitometric method were statistically compared to those obtained by the reported HPLC methods and no significant difference was found between them.

scholarly journals Magnetic-Dispersive Solid Phase Extraction Based on Graphene Oxide–Fe3O4 Nanocomposites Followed by High Performance Liquid Chromatography-Fluorescence for the Preconcentration and Determination of Terazosin Hydrochloride in Human Plasma

2019 ◽  
Vol 58 (2) ◽  
pp. 178-186 ◽  
Author(s):  
Yaser Pashaei ◽  
Bahram Daraei ◽  
Maryam Shekarchi
Keyword(s):  
High Performance Liquid Chromatography ◽  
Graphene Oxide ◽  
Human Plasma ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction ◽  
Plasma Samples ◽  
Dispersive Solid Phase Extraction ◽  
X Ray

Abstract In the present study, a facile modified impregnation method was employed to synthesize superparamagnetic graphene oxide–Fe3O4 (GO–Fe3O4) nanocomposites. Based on the GO–Fe3O4 as adsorbent, a simple and fast magnetic-dispersive solid phase extraction followed by high performance liquid chromatography with fluorescence detection (M-dSPE–HPLC–FL) method was established and validated for the preconcentration and determination of terazosin hydrochloride (TRZ) in human plasma samples. The obtained nanomaterials were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy and vibrating sample magnetometry. Different parameters affecting the extraction efficiency, such as sample pH, amount of sorbent, extraction time, elution solvent and its volume and desorption time, were evaluated and optimized. The linearity of the proposed method was excellent over the range 0.3–50.0 ng mL−1 with an acceptable coefficient of determination (R2 = 0.9989). The limit of quantification and limit of detection were found to be 0.3 and 0.09 ng mL−1, respectively, and the preconcentration factor of 10 was achieved. Intra- and inter-day precision expressed as relative standard deviation (RSD %, n = 6) were between 2.2–3.8% and 4.7–6.4%, respectively. Accuracy, estimated by recovery assays, was 97.7–106.6% with RSD ≤ 5.2%. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of TRZ in human plasma samples.

Liquid-chromatographic determination of serotonin in serum and plasma.

1978 ◽  
Vol 24 (9) ◽  
pp. 1509-1514 ◽  
Author(s):  
S Sasa ◽  
C L Blank ◽  
D C Wenke ◽  
C A Sczupak
Keyword(s):  
High Performance ◽  
Clinical Laboratory ◽  
Chromatographic Determination ◽  
Present Scheme ◽  
Long Term Storage ◽  
Significant Difference ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Using high-performance liquid chromatography with electrochemical detection, we determined serotonin in plasma from parkinsonian patients being treated with L-3,4-dihydroxyphenylalanine or N-(DL-seryl)-N'(2,3,4-trihydroxybenzyl)hydrochloride plus L-3,4-dihydroxyphenylalanine ("Sinemet") and in serum from a blood bank, from "normal" persons, and a pooled specimen from a hospital clinical laboratory. The values obtained for the two groups of Parkinson's disease patients showed no significant difference. Long-term storage on solid CO2 was xhown to be an adequate technique for preserving samples. The mean (+/-SEAM) normal value obtained for serotonin in serum was 146 +/- 46 microgram/liter (n = 23), a result in harmony with that previously obtained [Clin. Chem. 20, 812 (1974)] by fluorometry. In comparison to other methods for measurement of serotonin in serum or plasma, we believe that the present scheme offers greater selectivity, sensitivity, and precision.

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