Stability of Fumonisins in Thermally Processed Corn Products†

1998 ◽  
Vol 61 (8) ◽  
pp. 1030-1033 ◽  
Author(s):  
MAURICIO M. CASTELO ◽  
SUSAN S. SUMNER ◽  
LLOYD B. BULLERMAN

Little is known about the stability of fumonisins in corn-based foods during heating. This study investigated the effects of canning, baking, and roasting (dry heating) processes on the stability of fumonisins in artificially contaminated and naturally contaminated corn-based foods. All samples were analyzed for fumonisin levels by both a commercial enzyme-linked immunosorbent assay (ELISA) and a high-performance liquid chromatographic (HPLC) method. Canned whole-kernel corn showed a significant (P ≤ 0.05) decrease in fumonisins by both ELISA (15%) and HPLC (11%) analyses. Canned cream-style com and baked corn bread showed significant (P ≤ 0.05) decreases in fumonisin levels at an average rate of 9% and 48%, respectively, as analyzed by ELISA. Corn-muffin mix artificially contaminated with 5 μg of fumonisin B1 (FB1,) per g and naturally contaminated corn-muffin mix showed no significant (P ≤ 0.05) losses of fumonisins upon baking. Roasting cornmeal samples artificially contaminated with 5 μg of FB1, per g and naturally contaminated commeal samples at 218°C for 15 min resulted in almost complete loss of fumonisins.

2010 ◽  
Vol 93 (4) ◽  
pp. 1228-1235 ◽  
Author(s):  
Mohamed Walash ◽  
Mohamed Metwally ◽  
Manal Eid ◽  
Rania El-Shaheny

Abstract A micellar HPLC method was developed for analysis of the antiosteoporosis drug risedronate. The analysis was carried out using a 250 4.6 mm id, 5 m particle size C18 Waters Symmetry column. The mobile phase consisted of 0.02 M sodium dodecyl sulfate + 0.3 triethylamine + 10 n-propanol, prepared in 0.02 M orthophosphoric acid. The pH of the mobile phase was adjusted to pH 6.0, and it was pumped at a flow rate of 0.7 mL/min with UV detection at 262 nm. The method showed good linearity in the range of 280 g/mL, with an LOD of 0.40 g/mL (1.31 106 M) and an LOQ of 1.21 g/mL. The suggested method was successfully applied for the analysis of risedronate in raw material and a tablet formulation, with average recoveries of 99.91 1.30 and 101.52 0.30, respectively. The stability-indicating capability of the proposed method was proved using forced degradation. By changing the pH of the mobile phase to 4.0, the oxidative degradation product could be separated from risedronate.


2006 ◽  
Vol 1 ◽  
pp. 117739010600100 ◽  
Author(s):  
Mohamed M. Hefnawy ◽  
Maha A. Sultan ◽  
Mona M. Al-Shehri

A high-performance liquid chromatographic (HPLC) method has been developed for the separation and determination of S- and R-enantiomers of betaxolol in tablets and ophthalmic preparations. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with fluorescence detection at excitation/emission wavelengths 275/305 nm. The polar ionic mobile phase (PIM) consists of methanol-glacial acetic acid-triethylamine, (100:0.020:0.025, v/v/v) has been used at a flow rate of 1.5 ml/min. All analytes with S-(-)-atenolol as internal standard were conducted at ambient temperature. The method is highly specific where another coformulated compounds did not interfere. The stability of betaxolol enantiomers under different degree of temperature also studied. The results showed that it is stable for at least 7 days at 70°C. The method validated for its linearity, accuracy, precision and robustness. Experimental design was used during validation to evaluate method robustness. Using the chromatographic conditions described, S- and R-betaxolol were well resolved with mean retention times of 11.3 and 12.6 min, respectively. Linear response (r > 0.997) was observed over the range of 10-500 ng/ml of betaxolol enantiomers, with detection limit of 5 ng/ml. The recoveries of S- and R-betaxolol from tablets and ophthalmic preparation ranged from 97.4 to 101.4% and 98.0 to 102.0%, respectively. The mean relative standard deviation (R.S.D.%) for both enantiomers were 1.1-1.4% and 1.3-1.7% in tablets and ophthalmic solution, respectively.


2011 ◽  
Vol 8 (s1) ◽  
pp. S41-S46
Author(s):  
Prafulla Kumar Sahu ◽  
M. Mathrusri Annapurna ◽  
Dillipkumar Sahoo

This paper describes a high-performance liquid chromatographic method for simultaneous estimation of nabumetone and paracetamol in binary mixture. The method was based on RP-HPLC separation and quantitation of the two drugs on hypersil C-18 column (250 mm × 4.6 mm) using a mobile phase consisting of acetonitrile and 0.05% aqueous acetic acid (70:30v/v) at flow rate of 1 mL min-1. Quantitation was achieved with PDA detector at 238 nm based on peak area with linear calibration curves at concentration ranges 5-25 µg mL-1for both the drugs. Naproxen sodium was used as internal standard. The method has been successively applied to pharmaceutical formulation. No chromatographic interference from the tablet excipients was found. The method was validated in terms of precision, robustness, recovery and limits of detection and quantitation. The intra and inter-day precision and accuracy values were in the acceptance range as per ICH guidelines.


INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (07) ◽  
pp. 32-37
Author(s):  
Vijaya Lakshmi Marella ◽  
Chaitanya S. N ◽  

A selective and sensitive reverse phase High Performance Liquid Chromatographic method has been developed and validated for the estimation of lornoxicam in bulk, pharmaceutical dosage forms and in dissolution samples. The analysis was performed isocratically on an Inertsil column (250* 4.6 mm, 5 µm) using a mass spectrometric compatible mobile phase of 10 mM ammonium acetate: acetonitrile (50:50 V/V) at a flow rate of 1 mL/min.The detection wavelength was 290 nm. The retention time was found to be 4.573 min for lornoxicam. The linearity of the method has been satisfied with Beer Lambert’s law in the concentration range of 5-25 µg/mL with a correlation coefficient of 0.9988. The mean recoveries assessed for lornoxicam were in the range of 100.39-101.86 %, indicating good accuracy of the method. The limit of detection and limit of quantification were found to be 0.03 and 0.11 µg/mL, respectively. The developed method has been statistically validated in accordance with ICH guidelines and found to be mass spectrometric compatible, simple, precise, and accurate with the prescribed values. Thus, the proposed method was successfully applied for the estimation of lornoxicam in routine quality control analysis of bulk, formulations and in dissolution samples.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (05) ◽  
pp. 48-52
Author(s):  
A Lodhi ◽  
◽  
A Jain ◽  
B. Biswal

A validated high performance liquid chromatographic method was developed for the determination of chromium picolinate in pharmaceutical dosage forms. The analysis was performed at room temperature using a reversed-phase ODS, 5µm (250×4.6) mm column. The mobile phase consisted of acetonitrile: buffer (60:40 V/V) at a flow rate of 0.5 mL/min. The PDA-detector was set at 264 nm. The developed method showed a good linear relationship in the concentration range from 1.5 – 12.5 µg/mL with a correlation coefficient from 0.999. The limit of detection and limit of quantification were 0.0540513 and 0.1637919 µg/mL respectively.


2013 ◽  
Vol 2013 ◽  
pp. 1-4
Author(s):  
Suying Ma ◽  
Haixia Lv ◽  
Xiaojun Shang

A high performance liquid chromatographic (HPLC) method with UV detector for the determination of dyclonine hydrochloride and a gas chromatography (GC) method with flame ionization detector (FID) for the determination of camphor and menthol in lotion were developed. The developed HPLC method involved using a SinoChoom ODS-BP C18reversed-phase column (5 μm, 4.6 mm × 200 mm) and mobile phase consisting of acetonitrile : water : triethylamine in a ratio of 45 : 55 : 1.0; pH was adjusted to 3.5 with glacial acetic acid. The developed GC method for determination of camphor and menthol involved using an Agilent 19091J-413 capillary chromatographic column (30 m × 320 μm × 0.25 μm). The two methods were validated according to official compendia guidelines. The calibration of dyclonine hydrochloride for HPLC method was linear over the range of 20–200 μg/mL. The retention time was found at 6.0 min for dyclonine hydrochloride. The calibration of camphor and menthol of GC method was linear over the range of 10–2000 μg/mL. The retention time was found at 2.9 min for camphor and 3.05 min for menthol. The proposed HPLC and GC methods were proved to be suitable for the determination of dyclonine hydrochloride, camphor, and menthol in lotion.


2010 ◽  
Vol 9 (8) ◽  
pp. 1260-1265 ◽  
Author(s):  
Elamin M Eid Eltayeb ◽  
Bustamam Abdul Ahmad ◽  
S Al Zubairi Adel ◽  
Aspollah Sukari Mohamed ◽  
Abdullah Rasedee

Author(s):  
Bryan J Starkey ◽  
Ian D R Fry

A new commercial enzymic kit for urinary oxalate determination has been adapted for use on a centrifugal analyser. It has been evaluated and compared with an established high performance liquid chromatographic (HPLC) procedure developed in our laboratory. Mean recovery of oxalate from urine samples augmented with oxalic acid exceeded 97% by both methods. The precision of the HPLC method was superior to that of the enzymic kit but both methods gave between batch precision values better than CV 12% at low (less than 100μmol/L) oxalate concentrations and better than CV 7% at higher concentrations (greater than 270μmol/L) Urinary oxalate values obtained with the new enzymic procedure correlated more closely with HPLC values ( r = 0·84) than did values previously obtained using the forerunner of the kit ( r = 0·62) which was known to be susceptible to ascorbate interference. No significant interference from ascorbic acid or from high urinary calcium concentrations could be demonstrated using either the improved kit or the HPLC procedure. Its easy adaptation to automated analysers available in most laboratories, coupled to its acceptable analytical performance render the enzymic kit a reasonable alternative to HPLC or other more complex procedures for urinary oxalate analysis.


INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 63-68
Author(s):  
R. Raut ◽  
◽  
A. Patil ◽  
V. K Munipalli ◽  
M. Patel ◽  
...  

A simple precise and rapid Reverse Phase High Performance Liquid Chromatographic (RP-HPLC) method has been developed for quantitative determination of Regorafenib in tablet dosage form. In this method Hypersil Gold (C18, 150mm× 4.6mm id, 3μ) column with mobile phase consisting of Trifluoroacetic acid (0.2% v/v) and Acetonitrile in the ratio of (50: 50 v/v) at 400C in an isocratic mode was used. The detection was carried out at 260 nm and 20μL injection volume was selected with the flow rate 1mL/min. The linearity range of Regorafenib shows concentration between 5-200 μg/mL. The regression coefficient obtained was 0.999. Retention time of Regorafenib was found to be 6.49 minutes. Acetonitrile and Water in the ratio of (3:1) was used as a diluent. The method was validated as per ICH guidelines and is simple, fast, accurate, precise and can be applied for routine quality control analysis of Regorafenib in tablet dosage form.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.


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