scholarly journals Variation of Deoxynivalenol Levels in Corn and Its Products Available in Retail Markets of Punjab, Pakistan, and Estimation of Risk Assessment

Toxins ◽  
2021 ◽  
Vol 13 (5) ◽  
pp. 296
Author(s):  
Shahzad Zafar Iqbal ◽  
Ahmad Faizal Abdull Razis ◽  
Sunusi Usman ◽  
Nada Basheir Ali ◽  
Muhammad Rafique Asi
Keyword(s):  
High Performance ◽  
Hazard Quotient ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Retail Markets ◽  
Significant Difference ◽  
Corn Products ◽  
Kolmogorov Smirnov ◽  
Natural Incidence ◽  
The Eu

This study investigated the natural incidence of deoxynivalenol (DON) in corn and corn products from corn-producing districts of Punjab, Pakistan. The analysis was carried out using high performance liquid chromatography (HPLC) with UV detector and immunoaffinity cleanup columns. The detection limit (LOD) and limit of quantification were 25 and 50 µg/kg, respectively. A total of 1220 samples of corn and corn products were analyzed to detect DON, and 539 (44.2%) samples were observed to be contaminated with DON (n ≥ LOD). Furthermore, 92 (7.5%) samples of corn and corn products had DON levels that were higher than the proposed limits of the EU. The data are significantly different from a normal distribution of DON in samples of corn and corn products from different locations (p < 0.05) for Shapiro–Wilk and Kolmogorov–Smirnov values. However, a significant difference in DON levels was found between corn and corn-derived products (p ≤ 0.05). The lowest and highest exposures, and hazard quotient (HQ) values of 0.92 and 9.68 µg/kg bw/day, were documented in corn flour samples.

scholarly journals Variation of Deoxynivalenol levels in Corn and Its Products Available in Retail Markets of Punjab, Pakistan and Estimation of Risk Assessment

2021 ◽  
Author(s):  
Shahzad Zafar Iqbal ◽  
Ahmad Faizal Abdull Razis ◽  
Sunusi Usman ◽  
Nada Basheir Ali ◽  
Muhammad Rafique Asi
Keyword(s):  
Risk Assessment ◽  
Hazard Quotient ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Retail Markets ◽  
Significant Difference ◽  
Kolmogorov Smirnov ◽  
Natural Incidence ◽  
Estimation Of Risk ◽  
The Eu

The study focused on investigating the natural incidence of deoxynivalenol (DON) in corn and products from corn producing districts of Punjab, Pakistan. The analysis was carried out using HPLC with UV detector and immunoaffinity cleanup columns. The detection limit (LOD) and limit of quantification were 25 and 50 &micro;g/kg, respectively. Total 1220 samples of corn and products were analyzed to detect the DON, and 539 (44.2%) samples were observed to be contaminated with DON (n &ge; LOD). Furthermore, 92 (7.5%) samples of corn &amp; products have DON levels, elevated than the proposed limits of the EU. The data is significantly different from a normal distribution for DON in corn and products samples and from different locations (p &lt; 0.05) for Shapiro-Wilk and Kolmogorov-Smirnov values. However, a significant difference in DON levels was found between corn and corn derived-products types (p &le; 0.05). The lowest and highest exposure &amp; hazard quotient (HQ) of 0.92 and 9.68 &micro;g/kg bw/d were documented in cornflour samples.

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.

Pharmacokinetic comparison of two buprenorphine formulations after buccal administration in healthy male cats

2017 ◽  
Vol 20 (4) ◽  
pp. 312-318 ◽  
Author(s):  
Brett M Gulledge ◽  
Kristen M Messenger ◽  
Karen K Cornell ◽  
Heather Lindell ◽  
Chad W Schmiedt
Keyword(s):  
Liquid Chromatography ◽  
Maximum Concentration ◽  
High Performance ◽  
Plasma Concentrations ◽  
Area Under The Curve ◽  
Storage Condition ◽  
Healthy Male ◽  
Limit Of Quantification ◽  
Significant Difference ◽  
Extent Of Absorption

Objectives The objective of this study was to compare the pharmacokinetics of compounded and commercially available aqueous formulations of buprenorphine after a single buccal dose to healthy cats and to evaluate the concentrations of a compounded buprenorphine solution over 21 days when stored at room temperature (RT; 22–24°C) with exposure to light or when refrigerated at 4°C while protected from light. Methods Six young healthy male cats were administered single buccal doses of compounded and commercially available formulations of buprenorphine (0.03 mg/kg) using a randomized, blinded, two-period crossover design. Blood samples were obtained over a 24 h period and plasma buprenorphine concentrations were determined using ultra-high-pressure liquid chromatography with mass spectrometry detection. Three batches of the compounded formulation were stored at RT or 4°C and aliquots were evaluated over 21 days for buprenorphine concentration using high-performance liquid chromatography with fluorescence detection. Results Plasma concentrations of buprenorphine were above the limit of quantification up to 6 h in some cats and up to 3 h in all cats. The area under the curve was significantly less for the compounded formulation ( P = 0.004). A significant difference was not detected between formulations for time to maximum concentration ( P = 0.11), maximum concentration ( P = 0.06), half-life ( P = 0.88) and mean residence time ( P = 0.57). Buprenorphine concentration in the compounded formulation was not affected by storage condition or time and remained between 90% and 110% of the target concentration at all time points. Conclusions and relevance A buprenorphine solution prepared from sublingual tablets is absorbed after buccal administration in healthy cats. The extent of absorption is significantly less than that of the commercially available formulation. The compounded solution maintains an acceptable buprenorphine concentration for at least 21 days when stored at RT or refrigerated.

scholarly journals A Quantitative, Sensitive and Rapid Validated Analytical RP-HPLC Method for the Estimation of Dapagliflozin in Bulk and Pharmaceutical Dosage Formulations

2020 ◽  
Vol 11 (2) ◽  
pp. 2543-2548
Author(s):  
Gouru Santhosh Reddy ◽  
Animesh Bera ◽  
Madhurima Basak ◽  
Krishnaveni Nagappan ◽  
Ramalingam Peraman
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Current Method ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Rp Hplc ◽  
Pharmaceutical Industries ◽  
Liquid Chromatography Method

The present study is aimed to develop a linear, precise, and accurate RP-HPLC (Reverse Phase High-Performance Liquid Chromatography) method for the determination of dapagliflozin in the formulation. The method was accomplished on a C18 column (250×4.6mm; 5µm), & Samples were eluted using acetonitrile: water (40:60%v/v) delivered at a flow rate of 1.0ml/min with a chromatographic run time of 10 min. The eluents were observed utilizing a UV detector with a wavelength set at 277nm. The method that was developed resulted in the retention of dapagliflozin at 7.029minutes. Dapagliflozin through current method has shown linearity (r2 > 0.999) over the concentration range of 1-16 µg/ml. The percentage recovery was observed to be within the limits of 98-102%, demonstrating the accuracy of the method. Limit of detection (LOD) and limit of quantification (LOQ) were qualified at 0.049µg/ml and 0.1485µg/ml, respectively. A Linear, precise, accurate, simple, and rapid RP-HPLC method has been developed and validated for the evaluation of dapagliflozin in bulk drug and tablet dosage forms (5mg &10mg) according to ICH Q2(R1) rules. Additionally, the proposed method could be of use in quality control tests of dapagliflozin in pharmaceutical industries.

scholarly journals A NEW VALIDATED STABILITY-INDICATING DIRECT HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR THE DETERMINATION OF ROSIGLITAZONE ENANTIOMERS IN THE PRESENCE OF ITS DEGRADATION PRODUCTS

2019 ◽  
pp. 64-67
Author(s):  
BYRAN GOWRAMMA ◽  
SUBRAMANIYAN NAIYANAR MEYYANATHAN ◽  
BASAWAN BABU ◽  
NAGAPPAN KRISHNAVENI
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Complete Separation ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Liquid Chromatography Method

Objective: In the present study, an isocratic chiral reverse-phase high-performance liquid chromatography method was developed and the resolution of the drug and complete separation from its degradation products were successfully achieved. Methods: An isocratic method developed with a Phenomenex Lux 5 μ Cellulose 1 (150 mm×4.6 mm i.d., 5 μ) using UV detector at wavelength of 220 nm, with a mobile phase consisting of methanol:0.1% diethylamine (60:40% v/v) and a flow rate of 1 ml/min. The drug was subjected to alkaline, acidic, neutral, oxidative, and photolytic to apply stress conditions. The stressed samples were analyzed by the proposed method. Results: The described method was linear over the range of 3–7 μg/ml for R-enantiomer and 9–21 μg/ml of S-enantiomer, respectively. The limit of detection and limit of quantification of R and S enantiomers were found to be 0.56 μg/ml and 0.18 μg/ml, respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The developed method can be applied in the quality control of drug products.

DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR AMISULPRIDE IN BULK AND PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (04) ◽  
pp. 43-50
Author(s):  
K. M. L Manoja ◽  
◽  
B. M. Gurupadayya ◽  
S Srujana ◽  
L. V. Raaga ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Forced Degradation ◽  
Uv Detector ◽  
Limit Of Quantification

A simple, sensitive, rapid, robust and reproducible method for the determination of amisulpride using paracetamol as internal standard (IS) in bulk and pharmaceutical formulation was developed using reverse phase high performance liquid chromatographic method. The analysis was performed on C18 (250 4.6 mm, 5 mcm) column with a mobile phase consisting of 0.03 M potassium dihydrogen ortho phosphate buffer (pH 6.5), acetonitrile in the ratio of 67:33 (V/V) with a flow rate of 1 mL/min. The analyte was monitored with UV detector at 263 nm. In the developed method amisulpride elutes at retention time of 4.4 min and paracetamol (IS) at 3.3 min. The proposed method is having linearity in the concentration range from 10-100 mcg/mL of amisulpride. The method was validated with respect to system suitability, linearity, precision, limit of detection (LOD) and limit of quantification (LOQ), accuracy (recovery),ruggedness, robustness, stability, forced degradation studies (specificity). The proposed method can be readily utilized for bulk drug and pharmaceutical formulations of amisulpride.

scholarly journals A Stability Indicating Novel UPLC-PDA Method for the Estimation in Bulk and Capsule Dosage form of Isavuconazole Effective for Mucormycosis Caused by COVID-19 Pandemic

2021 ◽  
pp. 505-513
Author(s):  
Suman Acharyya ◽  
Si, Abhik ◽  
H. K. Sundeep Kumar
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Current Approach ◽  
Chromatographic Technique ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Alkaline Peroxide ◽  
Degradation Analysis ◽  
Liquid Chromatographic

The present research provides a new proven ultra-high-performance liquid chromatographic technique for isavuconazole in both bulk and capsule dosage forms. DIKMA Waters BEH C18(50 x 2.6mm, 1.7m) column was used for chromatographic separation. With the isocratic elution mode, a mixture phosphate buffer: methanol 40:60 v/v, was used as the mobile phase, and the eluent was measured at 253 nm using a UV detector. The strategy has been maintained and validated in accordance with the International Conference on Harmonization Guidelines. Stressed deterioration has also been investigated in acidic, alkaline, peroxide, thermal, and photolytic conditions. Isavuconazole was eluted with the retention time 0.861 minute in this procedure. The calibration curve plots for isavuconazole were found to be linear within the concentration ranges of 1-25µg/mL. With a percentage recovery of 100.18 percent, the limit of detection was 0.025g/ml and the value for limit of quantification was 0.50µg/mL. In a force degradation analysis, the current approach was also determined to be stable. Based on the experiential evidence, the present method was found appropriate of isavuconazole estimation in the form of bulk and capsule.

scholarly journals Determination of Oxalates in Corms of Selected Taro (Colocasia esculenta) Varieties in Malaysia Using Ultra High-Performance Liquid Chromatography

2020 ◽  
pp. 28-37
Author(s):  
A. Mohd Zulkhairi ◽  
M. Razali ◽  
M. B. Umikalsum ◽  
G. Mohd Norfaizal ◽  
A. Aimi Athirah ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Dry Weight ◽  
Peninsular Malaysia ◽  
Colocasia Esculenta ◽  
Uv Detector ◽  
Commercial Cultivation ◽  
Significant Difference ◽  
The Difference

Aims: To determine the oxalate contents in different varieties of taro (Colocasia esculenta) collected in Peninsular Malaysia. Study Design: Ultra High-Performance Liquid Chromatography (UHPLC) with UV detector (Diode Array Detection, (DAD)) was used to determine the total and soluble oxalate contents in different varieties of taro corms. Meanwhile, the insoluble oxalate content (calcium oxalate) was estimated from the subtraction of soluble oxalate content from total oxalate content. Place and Duration of Study: Malaysian Agriculture Research and Development Institute (MARDI Headquarters), Persiaran MARDI-UPM, 43400 Serdang, Selangor, Malaysia between December 2018 to December 2019. Methodology: 9 different varieties of taro were collected from different locations in Peninsular Malaysia. All the samples were analysed for their oxalate contents. Extractions were carried out to determine the total oxalate and soluble oxalate contents. All the samples were analysed using UHPLC. The generated data of oxalate contents were analysed using Analysis of Variance (ANOVA). Results: There is a significant difference (P <.05) between the oxalate content in the examined varieties with respect to the amount of total, soluble and insoluble oxalate contents. The putih variety has significantly the highest amount of total oxalate content with 218.8 ± 28.2 mg/100 g DW (dry weight) followed by the udang variety with 184.2 ± 24.7 mg/100 g DW and the wangi variety with 178.3 ± 5.1 mg/100 g DW. Tapak badak variety has the lowest total oxalate content with 70.5 ± 20.1 mg/100 g DW. Result showed that wangi variety has significantly the highest soluble oxalate content with 135.1 ± 4.8 mg/100 g DW followed by udang with 100.9 ± 49.8 mg/100 g DW. The lowest soluble oxalate content was found in tapak badak with 17.7 ± 2.9 mg/100 g DW. Conclusion: Despite many factors contributing to the difference in oxalate content between varieties, this study would help researchers or policy makers to suggest potential taros for commercial cultivation.

HPLC DETERMINATION OF N-METHYLETHANOLAMINE IN DIPHENHYDRAMINE HYDROCHLORIDE DRUG SUBSTANCE BY PRE-COLUMN DERIVATIZATION

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (10) ◽  
pp. 56-62
Author(s):  
A Anerao ◽  
◽  
V. Dighe ◽  
A Gupta ◽  
C. Patil ◽  
...  
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Diphenhydramine Hydrochloride ◽  
Liquid Chromatography Method

N-Methylethanolamine is the side chain of the drug diphenhydramine hydrochloride. A sensitive high performance liquid chromatography method with pre-column derivatization was developed and validated for the determination of N-methylethanolamine impurity in diphenhydramine hydrochloride active pharmaceutical ingredient. HPLC method on column Cosmosil MS-II, C-18, 250 mm X 4.6 mm, particle size 5 μm with UV detector was used. The proposed method is specific, linear, accurate, rugged and precise. The calibration curves showed good linearity over the concentration range of 0.03 mg/g to 1.5 mg/g and the correlation coefficient was 0.999. Method had very low limit of detection (LOD) and limit of quantification (LOQ) as 0.01 mg/g and 0.03 mg/g, respectively, of the analyte. Accuracy was observed within 94.4% to 96.2%.

scholarly journals Investigation a clean up procedure for chlorophenols in soil by ultrasonic and solid phase extraction

2019 ◽  
Vol 2 (2) ◽  
pp. 118-124
Author(s):  
Truong Vinh Doan ◽  
Vinh Xuan Le ◽  
Hien Thi To ◽  
Thuan Thi Ngo
Keyword(s):  
Risk Assessment ◽  
High Performance ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Clay Content ◽  
Soil Samples ◽  
Phase Extraction ◽  
Uv Detector ◽  
High Recovery ◽  
Limit Of Quantification

Chlorophenol is a group of toxic and presistent compounds in soil. Investigation on an appropriate procedure is very important to quantify all chlorophenol congeners. All parameters in ultrasonic combined with soild phase C18 extraction (SPE_C18), and then high performance liquid chromatography/ UV detector were selected and optimised. Various soil samples contaminated by chlorophenols containing from 0.67% to 2.36% of organic matter and clay content from 1.37%–22.30% were selected and examined. The results showed that a group of 3–chlorophenol, 3,4–dichlorophenol, 3,5–dichlorophenol, 3,4,5– trichlorophenol, 2,3,4,6–tetrachlorophenol, 2,3,4,5– tetrachlorophenol, pentachlorophenol contaminated in soils has high recovery efficiencies (>70%) with low standard devitation (<7%). This method is suitable to analyze chlorophenol in soil with limit of detection (LOD) about 0.2mg/kg and limit of quantification (LOQ) about 1mg/kg. This research is helpful in risk assessment of chlorophenols contaminated in soil and suitable in Vietnam.

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