Aflatoxins in cotton seeds and cotton seed cake from Pakistan.

A study was conducted to evaluate the natural occurrence of aflatoxins (AFB1, AFB2, AFG1, AFG2) in cotton seeds (n = 110) and cotton seed cake (CSC; n = 110) from Pakistan. All samples were screened by Enzyme-Linked ImmunoSorbent Assay (ELISA). Positive samples were further quantified by IAC-HPLC-FLD. Total contamination frequency and aflatoxins mean levels were 80% and 69 µg/kg in cotton seeds and the corresponding values for cotton seed cake 88% and 89 µg/kg, respectively. Aflatoxin B1was found in all positive samples and co-occurred with AFB2, AFG1, and AFG2. Sixty-four cotton seeds and 71 CSC samples contained aflatoxins levels higher than the ML set for animal feed (20 µg/kg). The results of the present study will help the regulatory authorities to formulate strategies for monitoring aflatoxins in animal feeds.

A simplified FTIR chemometric method for simultaneous determination of four oxidation parameters of frying canola oil.

Transmission Fourier transform infrared (FTIR) spectroscopic method using 100 µm KCl cell was applied for the determination of total polar compounds (TPC), carbonyl value (CV), conjugated diene (CD) and conjugated triene (CT) in canola oil (CLO) during potato chips frying at 180 °C. The calibration models were developed for TPC, CV, CD and CT using partial least square (PLS) chemometric technique. Excellent regression coefficients (R(2)) and root mean square error of prediction values for TPC, CV, CD and CT were found to be 0.999, 0.992, 0.998 and 0.999 and 0.809, 0.690, 1.26 and 0.735, respectively. The developed calibration models were applied on samples of canola oil drawn during potato chips frying process. A linear relationship was obtained between CD and TPC with a good correlation of coefficient (R(2)=0.9816). Results of the study clearly indicated that transmission FTIR-PLS method could be used for quick and precise evaluation of oxidative changes during the frying process without using any organic solvent.

Estimation of ibuprofen in urine and tablet formulations by transmission Fourier Transform Infrared spectroscopy by partial least square.

A rapid, reliable and cost effective analytical procedure for the estimation of ibuprofen in pharmaceutical formulations and human urine samples was developed using transmission Fourier Transform Infrared (FT-IR) spectroscopy. For the determination of ibuprofen, a KBr window with 500 µm spacer was used to acquire the FT-IR spectra of standards, pharmaceuticals as well as urine samples. Partial least square (PLS) calibration model was developed based on region from 1807 to 1,461 cm(-1) using ibuprofen standards ranging from 10 to 100 µg ml(-1). The developed model was evaluated by cross-validation to determine standard error of the models such as root mean square error of calibration (RMSEC), root mean square error of cross validation (RMSECV) and root mean square error of prediction (RMSEP). The coefficient of determination (R(2)) achieved was 0.998 with minimum errors in RMSEC, RMSECV and RMSEP with the value of 1.89%, 1.63% and 4.07%, respectively. The method was successfully applied to urine and pharmaceutical samples and obtained good recovery (98-102%).

Simultaneous assessment of zinc, cadmium, lead and copper in poultry feeds by differential pulse anodic stripping voltammetry.

In the present work four metals (Zn, Cd, Pb and Cu) were determined simultaneously in 28 commercial broiler poultry feeds by differential pulse anodic stripping voltammetry (DPASV) using hanging mercury drop electrode (HMDE). The digestion of poultry feeds was carried out with concentrated nitric acid and hydrogen peroxide (2:1) with the help of microwave heating. Acetate buffer of pH 5 was used as a supporting electrolyte. The limit of detection for Zn, Cd, Pb and Cu was 0.69, 0.35, 0.68 and 0.24 microg/kg, respectively. The amount of Zn, Cd, Pb and Cu in the analyzed poultry feeds was ranged between 54.3-482.2, 3.8-33.6, 23.2-32.6 and 12.3-65.8 mg/kg, respectively. In most of analyzed poultry feed samples, the amount of Cd and Pb was found to be greater than the maximum tolerable level (MTL) which could be harmful for the poultry.

A simplified UV spectrometric method for determination of peroxide value in thermally oxidized canola oil.

The aim of present study was to develop a simple method on UV spectrometer for the determination of peroxide value (PV) of the frying oil. The basis of the PV determination was the stoichiometric reaction of triphenylphosphine (TPP) with the hydroperoxides present in frying oil to produce triphenylphosphine oxide (TPPO), which exhibits a readily measurable absorption band at 240 nm by ultraviolet region. The PV ranged between 0.15 and 11.66 meq. of active oxygen per kilogram of oil as the canola oil was heated from 0 to 12h in the fryer at 180 degrees C. The proposed method was correlated with official AOCS titration method and best correlation coefficient (R(2)=0.99525) was achieved, proving that there is no significant difference in the results. Therefore, developed method could serve as an alternative to the titration method, for the determination of PV in frying oils.

Main fatty acid classes in vegetable oils by SB-ATR-Fourier transform infrared (FTIR) spectroscopy.

The prospect of using single bounce attenuated total reflectance (SB-ATR)-Fourier transform infrared (FTIR) spectroscopy as a rapid quantitative tool to determine the main fatty acid groups present in different edible oils was investigated. Partial least squares (PLS) calibrations were developed using SB-ATR-FTIR spectra which were associated with fatty acid groups (saturated, trans, mono- and polyunsaturated) using quantitative data obtained by gas chromatography (GC). Good calibrations were obtained for all main four fat groups (saturated, mono, trans and polyunsaturated) with excellent precision. The coefficient of determination (R(2)), root mean square error of prediction (RMSEP) and bias for validation set were obtained as 0.999, 2.43 and 0.998 for saturated; 0.999, 1.850 and 0.003 for mono; 0.999, 0.625 and -0.001 for trans while for poly the values were 0.999, 1.170 and 0.003, respectively. The results of 13 validation samples for total saturated, mono, trans and polyunsaturated fats by FI-IR were found in the range of 8.16-55.16, 37.62-74.75, 0.20-18.16 and 1.36-62.35%, respectively. The present study shows that it may well be possible to expand the utility of SB-ATR-FTIR spectroscopy not only to provide isolated trans data, but also serve as a simple, rapid and quantitative means of categorizing the main groups present in the edible oils. The information obtained would be useful for meeting the new lipid nutritional labeling requirements.

Application of microwave heating for the fast extraction of fat content from the poultry feeds.

A rapid method has been developed to extract and quantitatively measure the total oil content in poultry feeds using a domestic microwave oven. The optimized extraction procedure involves the replicate (6x) extraction of 5 g of ground feed with 12 ml of hexane for 20 s in a 900 W oven. Each replicate involves the collection of the resulting miscella and its replacement with fresh solvent for re-extraction. The collected extracts were centrifuged and transferred to a vial. The solvent was evaporated to a constant weight and the residual lipid weighed. In comparison to conventional Soxhlet extraction method, lipid contents obtained using the optimized microwave procedure was not significantly different. However, FTIR analysis indicated that the microwave procedure was superior in minimizing the formation of free fatty acids (FFA) relative to the Soxhlet procedure if the temperature of the sample was kept within the range of 45-50 degrees C. This simple, sequential extraction procedure is rapid, highly efficient and provides a simple mean of quantitating the lipid content of poultry feed in less than 40 min without the need for specialized microwave oven.

GC-MS quantification of fatty acid profile including trans FA in the locally manufactured margarines of Pakistan.

Ten margarine brands of Pakistan were analyzed for their fatty acid composition with emphasis on trans fatty acids (TFA) using GC-MS. Saturated, cis-monounsaturated and polyunsaturated fatty acids were present at 24.2-58.1, 5.7-35.4 and 3.8-37.4% of total fatty acids, respectively. Among the saturated fatty acids, palmitic acid (16.9-33.8%) was dominant in all analyzed margarine brands and its higher amount indicates that palm oil was a major contributor in the margarine manufacturing. Among samples tested only one contained a low level of TFA (2.2%) while the rest contained very high amounts of TFA (11.5-34.8%) which clearly shows that hydrogenated oils were used in the formulation of margarines. Fatty acid profiles demonstrated that all samples belong to the hard margarine category containing high amounts of trans and saturated fatty acids which is an alarming issue for the health of consumers.

Rapid determination of free fatty acids in poultry feed lipid extracts by SB-ATR FTIR spectroscopy.

A simple, rapid, and reproducible method has been developed for the quantitative determination of free fatty acid (FFA) content in lipids extracted from poultry feeds by Fourier transform infrared (FTIR) spectroscopy with the use of a single-bounce attenuated total reflectance (SB-ATR) accessory. An FTIR calibration curve was prepared by gravimetrically adding oleic acid (15-37%) to pure refined, bleached, and deodorized (RBD) canola oil and measuring the area of the COOH absorption band at 1710 cm-1. The oil from each of 12 poultry feed formulations was extracted using conventional Soxhlet extraction, and after evaporation of the solvent, the FFA content was determined by the conventional AOCS titrimetric procedure and by the SB-ATR/FTIR method. The SB-ATR/FTIR FFA predictions were related to those determined by the AOCS titrimetric method by linear regression, producing an R value of 0.999 and a SD of +/-0.28% FFA. Time-course spectra collected as lipids extracted into hexane indicated that a 15 min extraction was adequate to obtain a representative sample for FFA determination, with further extraction resulting in little, if any, change in the proportion of FFA in the lipid extract. Only a small volume of the hexane extract ( approximately 20 mL) yielded sufficient material for the SB-ATR/FTIR analysis. Thus, by shortening the extraction time and taking a small sample so as to reduce solvent removal time, the SB-ATR/FTIR procedure provides a very simple and rapid means of determining the FFA content of poultry feed lipids.