Assessment of pesticide residues in commonly used vegetables in Hyderabad, Pakistan.

The aim of present study was to assess pesticide residues in vegetables in the Hyderabad region of Pakistan. The concentrations of six pesticides were determined by gas chromatography coupled with mass selective detector (GC-MSD) in locally produced vegetables purchased from wholesale markets. A total of 200 samples of eight vegetables viz. cauliflower, green chilli, eggplant, tomato, peas, bitter gourd, spinach and apple gourd were analyzed for pesticide residues. The results indicated that almost all samples were contained pesticides, only 39% contained pesticide residues at or below maximum residue limits (MRLs), and 61% contained pesticide residues above MRLs. From the six analyzed pesticides, carbofuran and chlorpyrifos were found above to MRLs with concentrations ranging from 0.01-0.39 and 0.05-0.96 mg/kg, respectively. The results provided important information on the current pesticide contamination status of some commonly used vegetables and pointed an urgent need to control the use of some excessively applied and potentially persistent pesticides, such as carbofuran and chlorpyrifos.

Quantitative separation of oxytocin, norfloxacin and diclofenac sodium in milk samples using capillary electrophoresis.

A simple, sensitive and rapid method has been developed for simultaneous separation and quantification of three different drugs: oxytocin (OT), norfloxacin (NOR) and diclofenac (DIC) sodium in milk samples using capillary electrophoresis (CE) with UV detection at 220 nm. Factors affecting the separation were pH, concentration of buffer and applied voltage. Separation was obtained in less than 9 min with sodium tetraborate buffer of pH 10.0 and applied voltage 30 kV. The separation was carried out from uncoated fused silica capillary with effective length of 50 cm with 75 microm i.d. The carrier electrolyte gave reproducible separation with calibration plots linear over 0.15-4.0 microg/mL for OT, 5-1000 microg/mL for NOR and 3-125 microg/mL for DIC. The lower limits of detection (LOD) were found to be 50 ng/mL for OT, and 1 microg/mL for NOR and DIC. The method was validated for the analysis of drugs in milk samples and pharmaceutical preparations with recovery of drugs within the range 96-100% with RSD 0.9-2.8%.

Utilization of organic by-products for the removal of organophosphorous pesticide from aqueous media.

Sorption potential of rice (Oryza sativa) bran and rice husk for the removal of triazophos (TAP), an organophosphate pesticide, has been studied. The specific surface area were found to be 19+/-0.7 m(2)g(-1) and 11+/-0.8m(2)g(-1) for rice bran and rice husk, respectively. Rice bran exhibited higher removal efficiency (98+/-1.3%) than rice husk (94+/-1.2%) by employing triazophos solution concentration of 3 x 10(-5) M onto 0.2 g of each sorbent for 120 min agitation time at pH 6 and 303 K. The concentration range (3.2-32) x 10(-5) M was screened and sorption capacities of rice bran and rice husk for triazophos were computed by different sorption isotherms. The energy of sorption for rice bran and rice husk was assessed as 14+/-0.1 and 11+/-0.2 kJ mol(-1) and kinetics of the sorption is estimated to be 0.016+/-0.002 and 0.013+/-0.002 min(-1), respectively. Intraparticle diffusion rate was computed to be 4+/-0.8 and 4+/-0.9 nmol g(-1)min(-1/2). Thermodynamic constants DeltaH, DeltaS and DeltaG at varying temperatures (283-323 K) were also calculated.

Antioxidant potential of commercially available cumin (Cuminum cyminuml inn) in Pakistan.

Owing to increased safety concerns about synthetic antioxidants, exploitation of safer antioxidants based on natural origin is the focus of research nowadays. Cumin is a common spice and is used as a routine supportive cooking agent. Extracts of cumin were prepared in methanol, ethanol, dichloromethane and hexane by employing Soxhlet extraction apparatus. Determination of the total phenolic content, chelating activity, reducing power and free radical scavenging activity were taken as parameters for the assessment of antioxidant properties. The findings of this study suggest cumin to be a potent source of antioxidants. Results from the different parameters were in agreement with one another.

Synthesis, characterization and antioxidant activity copper-quercetin complex.

Quercetin (3,3',4',5,7-pentahydroxyflavone) one of the most abundant dietary flavonoids, has been investigated in the presence of Cu(II) in methanol. The spectroscopic studies (UV-vis, (1)H NMR and IR) were useful to assess the relevant interaction of Quercetin with Cu(II) ions, the chelation sites and dependence of the complex structure from the metal/ligand ratio. A 1:2 (L:M) complex was indicated by Job's method of continuous variation, which was applied to ascertain the stoichiometric composition of the complex. The antioxidant activities of the compounds were evaluated by using the 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging method. The complexed flavonoid was much more effective free radical scavengers than the free flavonoids.

Characterization of banana peel by scanning electron microscopy and FT-IR spectroscopy and its use for cadmium removal.

This study describes the use of banana peel, a commonly produced fruit waste, for the removal of Cd(II) from environmental and industrial wastewater. The banana peel was characterized by FT-IR and scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis. The parameters pH, contact time, initial metal ion concentration and temperature were investigated and found to be rapid ( approximately 97% within 10 min). The Langmuir adsorption isotherm was used to describe partitioning behavior for the system at room temperature. The value of Q(L) was found to be (35.52 mg g(-1)) higher than the previously reported materials. The binding of metal ions was found to be pH-dependent with the optimal sorption occurring at pH 8. The retained species were eluted with 5 mL of 5 x 10(-3)M HNO(3) with the detection limit of 1.7 x 10(-3)mg L(-1). Kinetics of sorption followed the pseudo-first-order rate equation with the rate constant k, equal to 0.13+/-0.01 min(-1). Thermodynamic parameters such as Gibbs free energy at 303K (-7.41+/-0.13 kJ mol(-1)) and enthalpy (40.56+/-2.34 kJ mol(-1)) indicated the spontaneous and endothermic nature of the sorption process. The developed method was utilized for the removal of Cd(II) ions from environmental and industrial wastewater samples using flame atomic absorption spectrophotometer (FAAS).

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.

Intramuscular fatty acid profile of longissimus dorsi and semitendinosus muscle from Pateri goats fed under traditional feeding system of Sindh, Pakistan.

The present study was undertaken to assess the intramuscular fatty acid composition of different muscles taken from male Pateri (n=15) goats, reared on naturally grown grasses, leaves and pods of Acacia nilotica and crushed cereal, under traditional way of feeding. Goats were slaughtered with an average weight of 68±7kg and age 12±1 month. The samples were taken from longissimus dorsi region (between the 12th and 13th rib) and distal region of semitendinosus muscle. Results of total fat content and fatty acids composition does not show significant (P>0.05) variation among muscles investigated. The fatty acid composition of muscles studied were primarily composed of oleic (31.50-33.38%), followed by palmitic acid (19.84-22.05%) and stearic acid (22.25-24.91%) respectively. Muscle tissue in general contained an average 51.13% of saturated fatty acids and 48.87% of unsaturated fatty acids. The mean conjugated linoleic acid was found 0.41%, 0.43% and 0.47% in ribeye and loin portion of longissimus dorsi muscle and distal region of semitendinosus muscle, respectively.

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.

The removal efficiency of chestnut shells for selected pesticides from aqueous solutions.

The removal of selected pesticides such as carbofuran (CF) and methyl parathion (MP) using low-cost abundant sorbent chestnut shells from aqueous solutions has been investigated in the present study. The sorption parameters, i.e., contact time, pH, initial pesticide solution concentration and temperature have been studied. Maximum percent sorption (99+/-1%) was achieved for (0.38-3.80) x10(-4) and (0.45-4.5) x10(-4) mol dm(-3) of MP and CF pesticide solutions respectively, using 0.4 g of sorbent in 100 ml of solution for 30 min agitation time at pH 6. The Freundlich, Langmuir and Dubinin-Radushkevich (D-R) models have been applied, and their constants for methyl parathion and carbofuran, sorption intensity 1/n (0.55+/-0.02 and 0.54+/-0.04), multilayer sorption capacity C(m) (28.3+/-0.5 and 16.4+/-0.7) x10(-3) mol l(1-1/n)dm(3/n)g(-1), monolayer sorption capacity Q (22.5+/-0.5 and 10.8+/-0.3) x10(-6) mo lg(-1), binding energy, b (2.9+/-0.2 and 5.2+/-0.5) x10(4) dm(3)mol(-1), and sorption energy E (11.2+/-0.1 and 11.5+/-0.2 kJ mol(-1)) have been evaluated respectively. Lagergren, Morris-Weber and Reichenberg equations were employed to study kinetics of sorption process. Thermodynamic parameters DeltaH (-5.09+/-0.1 and 22.8+/-0.4 kJ mol(-1)), DeltaS (-4.33+/-0.0003 and 0.09+/-0.001 kJ mol(-1)K(-1)) and DeltaG((303K)) (-2.9 and -3.8 kJ mol(-1)) have been calculated for methyl parathion and carbofuran, respectively. The developed sorption procedure has been employed to environmental samples.

Low cost sorbents for the removal of methyl parathion pesticide from aqueous solutions.

Sorptive potential of selected agricultural waste materials i.e. rice (Oryza sativa) bran (RB), bagasse fly ash (BFA) of sugarcane (Saccharum officinarum), Moringa oleifera pods (MOP) and rice husk (RH) for the removal of methyl parathion pesticide (MP) from surface and ground waters has been investigated. Optimization of operating parameters of sorption process, i.e. sorbent dose, agitation time, pH, initial concentration of sorbate, and temperature have been studied. The sorption data fitted to Freundlich, Langmuir and Dubinin-Radushkevich (D-R) sorption isotherms. The maximum capacities of RB, BFA, MOP and RH for MP were calculated to be 3.6+/-0.8, 5.3+/-1.4, 5.2+/-1.5 and 4.7+/-1.0 mmolg(-1) by Freundlich, 0.39+/-0.009, 0.39+/-0.005, 0.36+/-0.004 and 0.35+/-0.008 mmolg(-1) by Langmuir and 0.9+/-0.08, 1.0+/-0.10, 1.0+/-0.10 and 0.9+/-0.07 mmolg(-1) by D-R isotherms respectively, employing 0.1g of each sorbent, at pH 6, 90 min agitation time and at 303 K. Application of first order Lagergren and Morris-Weber equations to the kinetic data yielded correlation coefficients, close to unity. Thermodynamic parameters of sorption process, i.e. DeltaH, DeltaS and DeltaG were computed and their negative values indicated the exothermic and spontaneous nature of sorption process. The pesticide may be stripped by sonication with methanol, making the regeneration and reutilization of sorbents promising. The sorbents investigated exhibited their potential applications in water decontamination, treatment of industrial and agricultural waste waters.

Sorption potential of Moringa oleifera pods for the removal of organic pollutants from aqueous solutions.

Moringa oleifera pods Lamarck (Drumstick or Horseradish) is a multipurpose medium or small size tree from sub-Himalayan regions of north-west India and indigenous to many parts of Asia, Africa, South America, and in the Pacific and Caribbean Islands. Its pods (MOP) have been employed as an inexpensive and effective sorbent for the removal of organics, i.e., benzene, toluene, ethylbenzene and cumene (BTEC) from aqueous solutions using HPLC method. Effect of different parameters, i.e., sorbent dose 0.05-0.8g, 25cm(-3) agitation time 5-120min, pH 1-10, temperature 283-308K and concentration of sorbate (1.3-13)x10(-3), (1.1-11)x10(-3), (0.9-9)x10(-3), (0.8-8)x10(-3)moldm(-3), on the sorption potential of MOP for BTEC have been investigated. The pore area and average pore diameter of the MOP by BET method using nitrogen as a standard are calculated to be 28.06+/-0.8m(2)g(-1) and 86.2+/-1.3nm respectively. Freundlich, Langumir and Dubinin-Radushkevich (D-R) sorption isotherms were employed to evaluate the sorption capacity of MOP. Sorption capacities of BTEC onto MOP have been found to be 46+/-10, 84+/-9, 101+/-4, 106+/-32mmolg(-1) by Freundlich, 8+/-0.1, 9+/-0.1, 10+/-0.3, 9+/-0.1mmolg(-1) by Langumir and 15+/-1, 21+/-1, 23+/-2, 22+/-3mmolg(-1) by D-R isotherms respectively, from BTEC solutions at 303K. While the mean energy of sorption process 9.6+/-0.3, 9.2+/-0.2, 9.3+/-0.3, 9.5+/-0.4kJmol(-1) for BTEC is calculated by D-R isotherm only. Rate constant of BTEC onto MOP 0.033+/-0.003, 0.030+/-0.002, 0.029+/-0.002, 0.027+/-0.002min(-1) at solution concentration of 1.3x10(-3), 1.1x10(-3), 0.9x10(-3) and 0.8x10(-3)moldm(-3) and at 303K have been calculated by employing Lagergren equation. Thermodynamic parameters DeltaH -8+/-0.4, -10+/-0.6, -11+/-0.7, -11+/-0.7kJmol(-1), DeltaS -22+/-2, -26+/-2, -27+/-2, -29+/-3Jmol(-1)K(-1) and DeltaG(303K) -0.9+/-0.2, -1.9+/-0.2, -2.3+/-0.1 and -2.6+/-0.2kJmol(-1) were also estimated for BTEC respectively at temperatures 283-308K. The negative values of DeltaH, DeltaS and DeltaG suggest exothermic, stable (with no structural changes at solid-liquid interface) and spontaneous nature of sorption process under optimized conditions. MOP has been used extensively to accrue and then to preconcentrate benzene, toluene and ethylbenzene in wastewater sample.

Sawdust--a green and economical sorbent for the removal of cadmium (II) ions.

The ability of sawdust (treated and untreated) waste, a waste material derived from the commercial processing of cedrus deodar wood for furniture production, to remove/preconcentrate Cd(II) ions from aqueous solution was determined. Sorption was found to be rapid (approximately 97% within 8 min). The binding of metal ions was found to be pH dependent, optimal sorption accruing at around pH 4-8. Potentiometric titrations of sawdust revealed two distinct pK(a) values, the first having the value similar to carboxylic groups (3.3-4.8) and second comparable with that of amines (8.53-10.2) with the densities 1.99 x 10(-4) and 7.94 x 10(-5), respectively. Retained Cd(II) ions were eluted with 5 ml of 0.1 mol l(-1) HCl. Detection limit of 0.016 microg ml(-1) was achieved with enrichment factors of 120. Recovery was quantitative using sample volume of 600 ml. The Langmuir and D-R isotherm equations were used to describe partitioning behavior for the system at different temperatures. Kinetic and thermodynamic behavior of sawdust for Cd(II) ions removal was also studied.

Capillary gas chromatographic determination of phenylpropanolamine in pharmaceutical preparation.

Analytical procedure has been developed for the gas chromatographic determination of phenylpropanolamine (PPA) using trifluoroacetylacetone (FAA) as derivatizing reagent. Elution is carried out from the column HP-5 (30 mx0.32 mm i.d.) with film thickness 0.25 microm at initial column temperature 70 degrees C for 5 min, followed by heating rate 10 degrees C/min up to 120 degrees C. Injection port temperature was maintained at 270 degrees C. Nitrogen flow rate was 2 ml/min and detection was by FID. The linear calibration curve was obtained with 30-150 microg/ml PPA with detection limit of 6.0 microg/ml. The method was used for the determination of PPA from Sinutab and Tavegyl-D tablets. The relative standard deviation (R.S.D.) for the analysis of pharmaceutical preparation was obtained within 0.4-0.9%.

Antioxidant properties of methanolic extracts from leaves of Rhazya stricta.

Because of increased safety concerns about synthetic antioxidants, exploitation of cheaper and safer sources of antioxidants based on natural origin is the focus of research nowadays. Rhazya stricta is a medicinally important plant native to South Asia. Extraction of antioxidants was carried out in different solvent systems, i.e., water, 80% methanol, 70% ethanol, and diethyl ether. The methanolic extract exhibited the highest total phenolic content among the extracts; therefore for further studies the methanolic extract was employed. Antioxidant activity measurement in the linoleic acid system, metal chelating activity, reducing power, scavenging effect on 1,1-diphenyl-2-picrylhydrazyl free radical, and superoxide anion radical scavenging activity were taken as the parameters for assessment of antioxidant potential of methanolic extracts. Results were compared with alpha-tocopherol and the synthetic antioxidant butylated hydroxyanisole. The antioxidant potential of methanolic extracts of R. stricta leaves was comparable with previously exploited potent antioxidants and is strongly concentration dependent.

Sorption potential of rice husk for the removal of 2,4-dichlorophenol from aqueous solutions: kinetic and thermodynamic investigations.

The sorption potential of chemically and thermally treated rice husk (RHT) for the removal of 2,4-dichlorophenol (DCP) from aqueous solutions has been investigated. Sorption of DCP by rice husk was observed over a wide pH range of 1-10. The effect of contact time between liquid and solid phases, sorbent dose, pH, concentration of sorbate and temperature on the sorption of DCP onto rice husk has been studied. The pore area and average pore diameter of RHT by BET method are calculated to be 17+/-0.6 m2g-1 and 51.3+/-1.5 nm, respectively. Maximum sorption (98+/-1.2%) was achieved for RHT from 6.1x10(-5) moldm(-3) of sorbate solution using 0.1g of rice husk for 10 min agitation time at pH 6 and 303K, which is comparable to activated carbon commercial (ACC) 96.6+/-1.2%, but significantly higher than chemically treated rice husk (RHCT) 65+/-1.6% and rice husk untreated (RHUT) 41+/-2.3%. The sorption data obtained at optimized conditions was subjected to Freundlich, Langmuir and Dubinin-Radushkevich (D-R) isotherms. Sorption intensity 1/n (0.31+/-0.01) and sorption capacity multilayer C(m) (12.0+/-1.6 mmolg(-1)) have been evaluated using Freundlich sorption isotherm, whereas the values of sorption capacity monolayer Q (0.96+/-0.03 mmolg(-1)) and binding energy, b, (4.5+/-1.0)x10(4)dm(3)mol(-1) have been estimated by Langmuir isotherm. The Langmuir constant, b, was also used to calculate the dimensionless factor, R(L), in the concentration range (0.6-6.1)x10(-4) moldm(-3), suggesting greater sorption at low concentration. D-R sorption isotherm was employed to calculate sorption capacity X(m) (2.5+/-0.07 mmolg(-1)) and sorption energy E (14.7+/-0.13 kJmol(-1)). Lagergren and Morris-Weber equations were employed to study kinetics of sorption process using 0.2g of RHT, 25 cm(3) of 0.61x10(-4)moldm(-3) sorbate concentration at pH 6, giving values of first-order rate constant, k, and rate constant of intraparticle transport, R(id), (0.48+/-0.04 min(-1) and 6.8+/-0.8 nmolg(-1)min(-1/2), respectively) at 0.61x10(-4)moldm(-3) solution concentration of DCP, 0.1g RHT, pH 6 and 2-10min of agitation time. For thermodynamic studies, sorption potential was examined over temperature range 283-323 K by employing 6.1x10(-4)moldm(-3) solution concentration of DCP, 0.1g RHT at pH 6 and 10 min of agitation time and values of DeltaH (-25+/-1 kJmol(-1)), DeltaS (-61+/-4 Jmol(-1)K(-1)) and DeltaG(303K) (-7.1+/-0.09 kJmol(-1)) were computed. The negative values of enthalpy, entropy, and free energy suggest that the sorption is exothermic, stable, and spontaneous in nature.

Efficiency of rice bran for the removal of selected organics from water: kinetic and thermodynamic investigations.

The sorption efficiency of indigenous rice (Oryza sativa) bran for the removal of organics, that is, benzene, toluene, ethylbenzene, and cumene (BTEC), from aqueous solutions has been studied. The sorption of BTEC by rice bran is observed over a wide pH range of 1-10, indicating its high applicability to remove these organics from various industrial effluents. Rice bran effectively adsorbs BTEC of 10 microg mL(-1) sorbate concentration from water at temperatures of 283-323 +/- 2 K. The effect of pH, agitation time between solid and liquid phases, sorbent dose, its particle size, and temperature on the sorption of BTEC onto rice bran has been studied. The pore area and average pore diameter of rice bran by BET method are found to be 19 +/- 0.7 m(2) g(-1) and 52.8 +/- 1.3 nm. The rice bran exhibits appreciable sorption of the order of 85 +/- 3.5, 91 +/- 1.8, 94 +/- 1.4, and 96 +/- 1.2% for 10 microg mL(-1) concentration of benzene, toluene, ethylbenzene, and cumene, respectively, in 60 min of agitation time using 0.1 g of rice bran at pH 6 and 303 K. The sorption data follow Freundlich, Langmuir, and Dubinin-Radushkevich (D-R) models. Sorption capacities have been computed for BTEC by Freundlich (32 +/- 3, 61 +/- 14, 123 +/- 28, and 142 +/- 37 m mol g(-1)), Langmuir (6.6 +/- 0.1, 7.5 +/- 0.13, 9.5 +/- 0.22, and 9.4 +/- 0.18 m mol g(-1)), and D-R isotherms (11 +/- 0.5, 16 +/- 1.3, 30 +/- 2.2, and 33 +/- 2.5 m mol g(-1)), respectively. The Lagergren equation is employed for the kinetics of the sorption of BTEC onto rice bran and first-order rate constants (0.03 +/- 0.002, 0.04 +/- 0.003, 0.04 +/- 0.003, and 0.05 +/- 0.004 min(-1)) have been computed for BTEC at their concentration of 100 mug mL(-1) at 303 K. Studies on the variation of sorption with temperatures (283-323 K) at 100 mug mL(-1) sorbate concentration gave thermodynamic constants DeltaH (kJ mol(-1)), DeltaG (kJ mol(-1)), and DeltaS (J mol(-1) K(-1)). The results indicate that the sorption of organics onto rice bran is exothermic and spontaneous in nature under the optimized experimental conditions selected. This sorbent has been used successfully to accumulate and then to determine benzene, toluene, and ethylbenzene in wastewater sample.

Enrichment of Pb(II) ions using phthalic acid functionalized XAD-16 resin as a sorbent.

A simple and reliable method has been developed using polymeric material containing phthalic acid as a chelating agent to concentrate ultratrace amounts of lead ions in aqueous solutions. After characterization by CHN, IR, and thermal studies, the static and dynamic sorption behavior of Pb(II) ions onto new synthetic resin has been investigated. The sorption has been optimized with respect to pH, shaking speed, and contact time between the two phases. Maximum sorption is achieved from solution of pH 5-8 after 10 min agitation time. The lowest concentration for quantitative recovery is 5.8 ng cm(-3) with a preconcentration factor of approximately 850. The kinetics of sorption follows the first-order rate equation with the rate constant k=0.58+/-0.04 min(-1). The variation of the equilibrium constant K(c) with temperature between 10 and 50 degrees C yields values of DeltaH, 52.4+/-1.65 kJmol(-1), DeltaS, 186+/-5.21 Jmol(-1)K(-1), and DeltaG(303K), -4.15+/-0.002 kJmol(-1). The sorption data of Pb(II) ions in the concentration range from 2.41x10(-6) to 1.44x10(-4) molL(-1) follows the Langmuir, Freundlich, and Dubinin-Radushkevich (D-R) isotherms at all temperatures investigated. The sorption of Pb(II) ions onto synthesized resin in the presence of common anions and cations has also been measured. The possible sorption mechanism of Pb(II) ions onto phthalic acid modified XAD-16 is also discussed. The sorption procedure is utilized to preconcentrate Pb(II) ions prior to their determination in automobile exhaust particulates by atomic absorption spectrometry using direct and standard addition methods.

Occurrence of ochratoxin A in poultry feeds and feed ingredients from Pakistan.

A study was conducted to evaluate the occurrence of ochratoxin A (OTA) in complete poultry feeds (n=80) and poultry feed ingredients (n=286) from Pakistan. All samples were first analyzed by indirect enzyme linked immunosorbent assay (ELISA), samples with OTA concentrations above the European Union maximum regulatory limit (MRL, 100 µg/kg) were further confirmed by HPLC-FLD. Contamination frequency and mean OTA levels were 31% and 51 µg/kg in feed ingredients, and the corresponding values for complete feeds were 38% and 75 µg/kg. Ten samples of complete poultry feed and 19 samples of feed ingredients contained OTA at levels higher than the MRL. The results of the present study indicate that there is a strong need for a more intense monitoring programs for OTA in poultry feed.

Gas and liquid chromatography of metal chelates of pentamethylene dithiocarbamate.

Capillary GC and HPLC of metal chelates of pentamethylene dithiocarbamate were examined. Copper(II), nickel(II), cobalt(III), iron(III), manganese(II) and chromium(III) chelates formed in slightly acidic media (pH 5) were extracted in methyl isobutyl ketone or chloroform. Capillary GC elution and separation was carried out on methylsilicone DB-1 column (25 m x 0.2 mm I.D.) with film thickness 0.25 microm. Electron-capture detection was used. Elution was carried at initial column temperature 200 degrees C with an increment at a rate of 5 degrees C/min up to 250 degrees C and maximum temperature was maintained for 10 min. Symmetrical peaks with baseline separation were obtained with the metal chelates investigated with linear calibration range between 5 and 25 microg/ml for each metal ion and detection limits in the range of 0.5-6.0 microg/ml corresponding to 27-333 pg of metal ion reaching to the detector. HPLC separation was carried out from LiChrosorb ODS, 5 microm column and complexes eluted with methanol-water-1 mM sodium acetate (70:28:2, v/v) with a flow-rate of 1.2 ml/ml. UV detection was at 260 nm. The detection limits obtained were in the range 2-6 microg/ml. The methods were applied to the determination of metal ions in canal water and coal samples with RSD values within 4.15%. The results when compared with a standard flame atomic absorption spectrophotometric method and revealed no significant difference.