Pakistan Journal of Analytical & Environmental Chemistry
Pakistan Journal of Analytical & Environmental Chemistry is biannual publication by National Centre of Excellence in Analytical Chemistry, University of Sindh, Jamshoro. Journal covers fields of pure and applied analytical chemistry, environmental, material, agricultural and food chemistry, geochemistry, biotechnology, pharmaceutical and biomedical sciences, development and modification of instruments and techniques with potentials in environmental sciences. The Journal started publishing in year 2000 with the title, 'Pakistan Journal of Analytical Chemistry', later title was changed to its current in the year 2006. ISSN: 1996-918X; E-ISSN:2221-5255.
National Centre of Excellence in Analytical Chemistry, University of Sindh
Analytical Method Development and Validation of High-Performance Liquid Chromatography for SimultaneousDetermination of Ibuprofen and Baclofen
Combining baclofen with ibuprofen offers synergistic pain relief by targeting both muscle spasms and inflammation, enhancing efficacy in managing musculoskeletal conditions. This study aims to develop and validate an analytical method for the separation and simultaneous determination of ibuprofen and baclofen in combination using high-performance liquid chromatography (HPLC) in pharmaceutical dosage forms. An HPLC analytical method was developed to simultaneously quantify ibuprofen and baclofen. The optimized method was validated in accordance with the International Conference on Harmonization (ICH) guidelines. The method was tested for validation parameters, including specificity, accuracy, precision, linear range, limit of detection, lower limit of quantification, and robustness. A simple HPLC method was developed to separate two active ingredients using a C18 stationary phase column (25 cm × 0.46 cm, 5 μm). The mobile phase consisted of methanol: buffer (pH 3 ± 0.05), and acetonitrile in a ratio of 5:30:65 (%v/v). The analysis was performed at 25 °C with a 1.5 mL/min flow rate. A 20 μL sample volume was injected and detected at 265 nm. The validation method was specific, precise, and accurate. The average recovery of the two ingredients was 100.5% [99.1-102.0]. The repeated tests of the two compounds at different concentrations showed a percentage relative standard deviation (%RSD) of less than 1%. The method demonstrated linearity for both ibuprofen and baclofen, with an R² value of 0.99. The linearity range was 12.5-150 μg/mL for baclofen, and was 100-1800 μg/mL for ibuprofen. The lower limit of quantification (LLOQ) was 7 and 6 μg/mL for ibuprofen and baclofen, respectively. The limit of detection (LOD) was 2 μg/mL for both ingredients. The developed method is simple, rapid, precise, and accurate. It can be used for routine analysis of a combination of ibuprofen and baclofen in pharmaceutical dosage forms.
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Phytochemical Profiling, Antioxidant, Antibacterial, and Wound Healing Effects of Rosemary Oil Hydrogel
Rosmarinus officinalis L., a Mediterranean perennial herb, is well known for its antibacterial, antioxidant, anti-inflammatory, and wound-healing properties. This study investigates the phytochemical profile of R. officinalis, including glycosides, terpenoids, phenols, flavonoids, saponins, alkaloids, and tannins, along with its biological activities. Quantitative analysis revealed high levels of terpenoids (71.15 ± 0.18 mg/mL), tannins (26.32 ± 0.16 mg TTA/mL), phenolics (8.20 ± 0.001 mg GAE/mL), and flavonoids (0.1874 ± 0.002 mg QE/mL). Gas chromatography– mass spectrometry (GC-MS) identified a chemotype with low 1,8-cineole (1.77%) and a high concentration of 1,2-hexanediol (67.34%), which may enhance the formulation’s stability and suitability for medicinal and cosmetic applications due to its antimicrobial and humectant properties. The DPPH assay demonstrated strong antioxidant activity with an IC₅₀ value of 21.80 ± 0.56 μg/mL, which is more potent than ascorbic acid (IC₅₀ = 33.79 ± 0.33 μg/mL). Antimicrobial testing using the disc diffusion method showed moderate activity against Staphylococcus aureus (17.33 ± 0.45 mm at 50% concentration) and limited activity against Escherichia coli (12 mm at 50%) compared to gentamicin (24.3 mm and 23.1 mm, respectively). The rosemary oil hydrogel demonstrated a statistically significant improvement in wound contraction (66.87% ± 2.15% by Day 16, p< 0.05) in a Staphylococcus aureus-infected mouse model when compared to negative, placebo, and standard treatment groups. These results support the therapeutic potential of R. officinalis oil hydrogel for topical wound care, combining antimicrobial, antioxidant, and healing effects in a biocompatible formulation.
Rosemary oil, Phytochemical analysis, Total phenolic content, Total flavonoid content, Total tannin content, Antioxidant properties, Antibacterial activity, GC-MS, Animal studies
Comparative Study of Mass Transfer Limitation Steps in Bemacid Yellow and Methyl Red Biosorption: Investigation using Unique and Binary Resistance Models
In this study, brewery waste was employed as an adsorbent to remove two dyes: Bemacid Yellow (BY) and Methyl Red (MR). Optimal operational conditions were determined using the Bach mode. Kinetic data fitting was carried out using pseudo first and second order models. The results revealed that the pseudo second order model exhibited a better fit for both dyes, with a high determination coefficient (R2=0.99). The single resistance model demonstrated a positive correlation between the initial dye concentration (C0) and the external mass coefficient (kf) described by the empirical relationships: kfMR = 0.00044C0.650 and kf(by) = 0.0208C0.0330 for MR and BY dyes adsorption, respectively. According to the obtained results from the binary resistances diffusion model, it was determined that pore diffusion played a dominant role in the adsorption process of both dyes. This conclusion was supported by the observed increase in the film diffusion coefficient (Df) values. On the other hand, alternative formulas indicate that the adsorption processes of BY were primarily controlled by film diffusion. To summarize, the adsorption process of both dyes is influenced by two key steps: pore diffusion and film diffusion. This analysis provides insights into the significance of each parameter and their respective contributions to the overall adsorption mechanism.
Bemacid Yellow, Methyl Red, Kinetic models, Mass transfer, Binary resistance
Efficient Concurrent Analysis of Mesotrione, Atrazine, Benoxacor and S-Metolachlor in Herbicide Formulate: Developing and Validating a Reversed-Phased HPLC Method
An effective, simple and reliable simultaneous determination method for four active compounds, mesotrione, benoxacor, atrazine and S- metolachlor, in herbicide formulate was first-time developed and substantiated in current study using reversed-phased high performance liquid chromatography, following ICH guidelines. The chromatographic separation with fine resolution was conducted on a 5 μm C-18 column (L x id, 15 cm x 4.6 mm) using acetonitrile:water 70:30 (v/v) at 1.0 mL/min flow rate and wavelength 260 nm (UV detector). The retention times for mesotrione, atrazine, benoxacor and S-metolachlor were obtained as 1.90, 3.50, 3.95, and 5.10 min, respectively. Limits of detection of mesotrione, atrazine, benoxacor and S-metolachlor were found to be 2.57, 2.27, 1.28, and 1.32 μg/mL, whereas limits of quantitation were 7.80, 6.86, 3.86, and 4.01 μg/mL, respectively. The regression coefficients from calibration curves were ˃ 0.998 for all studied pesticides. The method reproducibility was evaluated as intra-day precision (0.85–1.52%RSD) and inter-day precision (0.67–1.81 %RSD). The method accuracy was estimated through inter-laboratory comparison among three laboratories. The developed method is quite rapid, inexpensive, robust, precise, accurate, linear and sensitive for the purpose of quality control check of mesotrione, atrazine, benoxacor and S-metolachlor simultaneously in herbicide formulations.
Crop protection agents, Liquid chromatography, Method optimization, Robustness, UV detector, System suitability
Municipal Solid Waste (Newspaper) — A Lignocellulosic Feedstock Conversion to Biofuel: A Prospective Solution to Energy and Waste Management Problem
Bioethanol, an alcohol-based fuel is produced from biowaste. The current research focuses on utilizing newspaper waste as a substrate for bioethanol production. The waste newspaper was pretreated and subjected to two important bioethanol production steps: (1) saccharification and (2) fermentation. Aspergillus niger utilized for the saccharification hydrolyzed the newspaper substrate by converting the complex compounds into simpler compounds, where lactose and chemically defined media enhanced the cellulolytic activity. The simpler sugars produced were fermented using the Saccharomyces cerevisiae and converted to bioethanol. The bioethanol samples were subject to different analyses, including dichromate oxidation tests, UV-Vis Spectroscopy, and High-Performance Liquid Chromatography (HPLC). The dichromate oxidation test confirmed the presence of bioethanol as the color of the samples changed from yellowish orange to green. The UV-Vis spectroscopy indicated the maximum bioethanol yield of 3.814% v/v (variant sample 1-lactose) and 5.049% v/v (variant sample 2-chemically defined media) on the 6th day of fermentation. HPLC further confirmed the bioethanol production as the peaks of bioethanol at retention times of 2.130 min (variant sample 1-lactose) and 2.112 min (variant sample 2-chemically defined media) matched the peak of standard ethanol at the retention time of 1.935 min. The present research concludes that newspaper waste is the potential substrate for bioethanol production.
Bioethanol, Newspaper, Waste management, Lignocellulose
Adsorption Studies of Cyanide (CN) - on Alumina
In this investigation, adsorption of cyanide on to alumina has been studied by means of batchtechnique. Percentage adsorption was determined for Alumina-Cyanide solution system as a function of (i) contact time, (ii) pH, (iii) adsorbate concentration and (iv) temperature. Adsorption data has been interpreted in terms of Freundlich and Langmuir equations. Thermodynamics parameters for the adsorption system have been determined at three different temperatures. The value of ΔHo=5.448kJ/mole and ΔGo=-7.162kJ/mole at 283K suggest that the adsorption of cyanide on Alumina is an endothermic and spontaneous process.
An Analytical Implication to Chlorides Determinationin Catalytic Hydrodechlorination Reaction of DDTby Ion Chromatography
Chemical degradation of Organochlorine pesticide (OCPs) in hydrodechlorination reactions were first systematically investigated using dichloro diphenyl trichloroethane (DDT) as the model pesticide. The reaction of DDT produced an equimolar amount of HCl and DDE resulting from initial attack and was identified using GC-ECD. The produced DDE was dechlorinated by using Fe/Ni catalysts with a solution of NaOH in 2-propanol/methanol (99:1 v/v) at temperature below 82 oC. The developed method efficiently converted DDT in the range of 3.5 – 3500 mg/l to chlorine-free product within 240 minutes. Chloride ions concentrations were also identified as a product using Ion Chromatography.
Chloride, Hydrodechlorination, DDT, Organochlorine pesticides
Evaluation of the Iodine Concentration in Serumand Urine of Hypothyroid Males Using anInexpensive and Rapid Method
The aim of present study was to evaluate the iodine/iodide status in biological samples (serum and urine) of 172 male hypothyroid patients (HPs) and their supplemental effects on thyroid hormones. For comparison purpose, non-goitrous subjects (n= 220) of same age group and socioeconomic status were also studied. A simple and rapid iodide-ion selective electrode (ISE) was used to measure the concentration of iodine in microwave assisted acid digested serum and urine samples. Quality control for the methodology was established with certified samples and with those obtained by conventional wet acid digestion method on the same certified reference materials (CRMs) and real samples. A linear calibration curve was obtained for a reasonable concentration range of the potassium iodide solutions. The mean concentration of iodine in the serum and urine samples of the HPs was significantly reduced as compared to control male subjects (p< 0.01). The low levels of free triiodothyronine and thyroxin were found in HPs than age matched healthy control (p< 0.005 and 0.002) respectively while high levels of thyroid stimulating hormone were observed in HPs (p< 0.008). The proposed method was relatively efficient as well as cost effective by using inexpensive equipment. It was observed that iodine in biological samples of HPs can play an important role in determining the severity of the hypothyroidism.
Iodine, male, hypothyroid, ion selective electrode, supplements
Effects of Chicken Frying on Soybean, Sunflower and Canola Oils
Consequences of discontinuous chicken frying on some important parameters of soybean (SBO), sunflower (SFO) and canola oil (CLO) at constant temperature (190 0C) for 12h were examined. The quality parameters such as fatty acid composition (FAC) with special emphasis on trans fatty acids (TFA’s), free fatty acids (FFA’s), iodine value (IV) and peroxide value (PV) of soybean, sunflower and canola oils were evaluated by taking out the oil samples from the fryer at an interval of 2 h. The total trans fatty acids increased during frying of chicken in the range of (0.77- 1.67, 1.02- 2.62 and 1.29-3.14 %) in SFO, SBO and CLO. Other chemical parameters such as free fatty acids (0.03-0.78, 0.05-0.49 and 0.19- 1.47 %), peroxide value (1.51-3.04, 2.11-6.07 and 2.90- 8.02 meq/kg) increased where as iodine value (154.21-140.69, 134.50 and 116.10-99.70 g/100g) was decreased with respect to time of frying in SFO, SBO and CLO, respectively.
chicken meat, frying, chemical parameters, fatty acid composition
Simpler and Faster Spectrophotometric Determination of Diclofenac Sodium in Tablets, Serum and Urine Samples
This work describes a simple, sensitive, rapid and economical analytical procedure for direct spectrophotometric evaluation of diclofenac sodium (DS) using aqueous medium without using a chemical reagent. Parameters like time, temperature, acidic and basic conditions and interference by analgesic drugs were studied for a 5μg ml-1 solution of DS at 276 nm. Under optimized parameters, a linear working range of 0.1–30 g ml-1 with regression coefficient of 0.9998 and lower detection limit of 0.01 g ml-1 was obtained. The method was applied for DS contents in tablets, serum and urine samples.
Diclofenac sodium; UV-Visible spectrophotometer; tablets; serum; urine
Determination of Toxic Metals in Different Brand of Chocolates and Candies, Marketed in Pakistan
In present study three toxic metals, cadmium (Cd), nickel (Ni) and lead (Pb) were determined in chocolates and candy samples available in local markets of Hyderabad, Pakistan. Concentrations of understudy toxic metals (TMs) were determined by electrothermal atomic absorption spectrometry (ETAAS) prior to microwave assisted acid digestion. Validation of the methodology was performed by standard addition method and conventional acid digestion on electric hot plate to obtained TMs concentration, for comparative purpose to obtain results within the 95% confidence level. No significant differences were observed for TMs obtained from both methods (P = 0.05). The concentration of Cd, Ni and Pb were observed in chocolates and candy samples is ranged as of 0.099 - 0.353, 1.45 - 4.33 and 1.11 - 2.48 μg/g, respectively. The results indicated that cocoa-based chocolates have higher contents of TMs than milk- based chocolates and candies.
Toxic metals, Chocolates, Candies, Atomic absorption spectrometry
Limnological Studies of Keenjhar Lake, District,Thatta, Sindh, Pakistan
Limnological studies of Keenjhar Lake were carried out during January 2003 to December 2005. The present study deals with physico - chemical parameters such as, temperature, pH, alkalinity, chlorides, conductivity, total dissolve solids, turbidity, dissolve oxygen, calcium and magnesium. The maximum and minimum range of physico - chemical properties were as, temperature 18 - 33 ⁰C from station 2 in January and August respectively, pH 7.3 - 8.9 in September and June respectively, alkalinity 160 - 240 mg L-1 in July and January respectively, minimum chlorides 30 mg L-1 in September and maximum 85 mg L-1 in December, conductivity 320 S cm-1 in September and 496 S cm-1 in December, total dissolve solids were 240 mg L-1 in September and 391 mg L-1 in October, turbidity was 30 NTU in December and 78 NTU in May, dissolve oxygen was 7.0 mg L-1 in January and 9.0 mg L-1 in July, calcium 50 mg L-1 in July and September and 78 mg L-1 in October, magnesium 21 mg L-1 in August and September, 35 mg L-1 June, and it is concluded that the variation in parameters were due to rain and flow of River Indus.
Physico - chemical properties, Keenjhar Lake, Thatta
Effect of Various Parameters on the Dispersionof Ultra Fine Iron Ore Slurry. Part-1
The effect of various dispersion parameters; such as slurry pH, solid concentration, stirring speed and time, and water quality has been extensively studied for stabilization the ultra fine iron ore slurry prior to selective flocculation. The PZC of Dilband iron ore system was found by using the Zetaphormeter III (CAD E400) at pH value of 4.25. The set of dispersion parameters was optimized on the basis of weight percent and the percent entrapment of fine particles (10μm) sedimented in 2.5min settling time. Finally the selectivity of the optimal dispersion parameters was evaluated on the basis of elemental analysis of the sediment. The optimal conditions for 38μm ultra fine iron ore slurry in double distilled water were found at concentration of 7.5%solid, pH10.5, stirring speed 2000rpm, and stirring time 5min.
Dilband iron ore, dispersion, zeta potential, polyvalent cations
Production of Ethanol by Indigenous Wild and MutantStrain of Thermotolerant Kluyveromyces Marxianus Under Optimized Fermentation Conditions
The maximum ethanol production and â-fructofuranocidase formation under fermentation studies were carried out in microprocessor controlled 23-L stainless steel fermenter at the following conditions: Temp = 40 ˚C (wild &mutant organism) , pH= 5.5, carbon source (molasses=15% sugar) nitrogen source (ammonium sulphate 0.75%), 300 RPM stirring speed and oxygen flow rate was 0.1 vvm. Mutant. Strain of thermotolerant Kluyveromyces marxianus M15 produced maximum production of ethanol at 48hr.All Kinetic Parameters have been studied for the utilization of substrate and production of maximum ethanol for both wild and mutant strains. It has been observed that wild strain was growing up to 550C while the mutant strain was growing up to 650C. In this comparison study, wild and mutant strain showed that Mutant-derived M15 was stronger over its parental culture due to its more thermal stability and production of ethanol at 65 oC at which wild organism could not grow.
Yeast, Fermentation, Kluyveromyces marxianus, metabolic network, thermal effects, Ethanol, Kinetic parameters
The Role of Paraquat (1,1-dimethyl-4,4-bipyridiniumchloride) and Glyphosate (n-phosphonomethyl glycine)in Translocation of Metal Ions to Subsurface Soils
We investigated the role of paraquat (1,1’-Dimethyl-4,4’-bipyridinium dichloride) and glyphosate (N-(phosphonomethyl) glycine), on the translocation of some metals (K, Mg(II), Mn(II), Fe(II), Pb(II), Cu(II) and Cd(II)) in soil, using a topsoil (Aquic Ustifluvent: USDA Soil Taxonomy, 2000) sampled at the University of Agriculture Makurdi Crop Farm, in Central Nigeria (7o 47’N, 8o 32’E). Employing column leaching experiments with water only on native soil and soil spiked with the metals and different levels of glyphosate or paraquat treatment, leachates were collected and analyzed for their metal contents. Results showed that in the presence of paraquat the transport of Fe(II) and Mn(II) by leaching in the soil was suppressed while that of Cu(II), K and Pb(II) was enhanced. Glyphosate, similarly suppressed Mn(II) and to some extent Fe(II) translocation in the soil; however, it enhanced the mobility of Cd(II), Cu(II), Mg(II), Pb(II) and K under similar treatment. While paraquat seemed to enhance the translocation of Mg(II) at low application rates of the herbicide, glyphosate promoted its transport only at high application rates; there was no evidence that paraquat affected the movement of Cd(II) in the soil. Our results show that the longterm use of these pesticides in the field may result in the depletion of Cu(II), K and Mg(II) in agricultural soils, and that the use of glyphospate may present the additional risk of possible groundwater contamination with Cd(II) and Pb(II).
Herbicide; Pesticide, Soil; Leaching; Leachate; Metal ion mobility; Glyphosate; Paraquat; Pollution; Nigeria
Peach-nut Shells-An Effective and Low Cost Adsorbent forthe Removal of Endosulfan from Aqueous Solutions
In the present studies the adsorption efficiency of peach nut shells for the removal of endosulfan from aqueous solutions has been investigated. The adsorption of endosulfan has been studied as a function of contact time, concentration and temperature. Maximum adsorption (95 ± 1%) was achieved for 0.24 × 10−4 mol dm−3 of endosulfan solution, using 0.1 g of adsorbent in 20 ml of solution for 30 min agitation time at pH 6. The Freundlich and Langmuir isotherms fit the equilibrium data satisfactory and their constants, adsorption intensity 1/n (0.36), multilayer adsorption capacity Cm 6.5 ± 0.26 mmol g−1, and monolayer adsorption capacity Q 0.27 ± 0.03 mmol g−1, have been evaluated. Thermodynamics parameters namely change in enthalpy ΔH, Gibbs free energy ΔG and entropy ΔS, were calculated. The negative values of ΔG and positive value of ΔH indicate that the adsorption process is spontaneous and endothermic in nature and positive value of entropy ΔS confirms the possibility of the favorable adsorption. The developed adsorption method has been employed to surface water samples.
Peach nut shells; Endosulfan; Adsorption; Isotherms; Thermodynamics
The Liquid-Liquid Extraction of Toxic Metals (Cd, Hg and Pb) by Calixarenes
Toxic metals (Cd, Hg and Pb) are mostly present in the environment due to natural phenomenon and human activities as well. Exposure of these non-essential elements in the environment causes severe effects. They are known to cause problems in humans as well as in aquatic life. In this work, we demonstrate various studies regarding liquid-liquid extraction of selected ions with different functionalized calixarenes. This review article briefly discusses several molecular designs of calixarenes for divalent ion (Cd2+, Hg2+ and Pb2+) recognition; as well as the relationship between structure and selectivity of the macrocycles is elaborated. The article does not, however, attempt to cover all of the different approaches to these toxic metal ions extraction
Calixarenes, Liquid-Liquid Extraction, Ion Recognition, Toxic Metals, Supramolecular Chemistry
Physico-chemical and Bacteriological Quality of Water from Shallow Wells in Two Rural Communities in Benue State, Nigeria
Ground water abstraction from shallow wells is widely practiced in the Obi and in Oju rural areas of Benue State, Central Nigeria, as a means of fighting guinea worm infestation associated with the surface water sources (streams) in these areas. To ascertain the physico-chemical and bacteriological quality of the water used by the population, water samples from 27 shallow wells in Obi and 19 Oju were taken and examined for key health-related quality parameters using routine methods. In Obi, the ground water colour ranged from 4.0-80.0 TCU, conductivity 55.2-1600.0 µS/cm, pH 6.1-8.6, TDS 38.6-1286 mg/L, turbidity 1.0-55.0 NTU, arsenic 0.001- 0.210mg/L, copper 0.01-2.53mg/L, fluoride 0.08-1.82mg/L and nitrate 10.8-63.0mg/L, while in Oju, colour varied from 2.0-87.0 TCU, conductivity 107.4-1375 µS/cm, pH 6.4-8.53, TDS 75.2- 1150 mg/L, turbidity 3.0-48.0 NTU, arsenic 0.001-0.023 mg/L, copper 0.01-2.10 mg/L, fluoride 0.01-1.54 mg/L and nitrate 10.2-59.7 mg/L. Some of these values in some instances exceed the WHO standard for drinking water. Alongside with the presence significant total coliform count in most of the wells (0-47/100 mL in Oju and 0-53/100 mL in Obi), the available water is considered largely unsafe for human consumption as obtained. It is concluded that, while ground water abstraction may be a safetymeasure against guinea worm infestation it, nevertheless presents other health challenges to the rural population in the area, as the quality of the ground water is generally low
Ground water, Shallow wells, Water quality, Rural community, Nigeria
Assay of Aliphatic Phthalates in Polymer Products by Sensitive Polarographic Method: Health and Environmental Issue
A faster, simpler and sensitive method was developed for determination of aliphatic phthalates using differential pulse polarography (DPP) as standard technique. The choice and concentration of base electrolyte, solvent, initial potential, effect of water addition and interference by other phthalates were the main parameters to optimize for enhancement of peak current and to obtain well-defined polarogram with lower background current using 1.3 x 10-4 M di-butyl phthalate (DBP) solution. Best results were obtained in the presence of tetra methyl ammonium bromide (TMAB) as electrolyte in methanol solvent with initial potential, -1.4 V. A linear calibration plot was observed in the range of 3 x 10-7 - 1.6 x 10-4 M DBP solution as aliphatic phthalates with lower detection limit of 5.9 x 10-8 M and linear regression coefficient of 0.9987. The developed polarographic method was successfully applied for analysis of aliphtaic phthalates in various samples of locally available polymer products such as baby toys, nipples, teethers, infusion blood bags and shopping bags. The results of the current method were compared with those obtained by a reported method and good agreement was found between them.
phthalates; Differential pulse polarography; Polymer products; Comparative method
Quantitative Analysis of Serum Lipid Profile in Gallstone Patients and Controls
The present study was undertaken to explore the possible role of serum lipid profile in gallstone formation. For this serum lipid profile such as total, free and bound cholesterol, LDL cholesterol, HDL cholesterol, triacylglycerols and total lipids were determined in 109 gallstone patients and 100 controls (matched for age, sex and with negative personal or family history of gallstones) treated at Liaquat University Hpspital, Jamshoro, Pakistan. Comparison for serum lipid profile between different groups of gallstone patients and controls revealed no significant variation except for the triacylglycerols and total lipids, which were differed significantly between females of up to 45 and above 45 years age. Comparison for serum lipid profile between pure cholesterol and mixed composition gallstone formers showed no significant difference (p>0.05) between the two groups. The serum lipid profile significantly varied between gallstone patients and controls except bound cholesterol level. Comparison of total cholesterol, free cholesterol, LDL cholesterol, HDL cholesterol, triacylglycerols and total lipids between gallstone patients and controls revealed that there was a significant difference between gallstone patients and controls for (a) females with or without gallstones, (b) females of up to 45 years age and (c) females having more than 3 children. HDL cholesterol is significantly decreased in all the groups of gallstone patients as compared to controls, whereas, bound cholesterol remained non significant in all the groups of gallstone patients when compared with controls. In conclusion, elevated serum total cholesterol, free cholesterol, LDL cholesterol, triacylglycerols and decreased levels of HDL cholesterolseem to play major contributing role in the pathogenesis of gallstones in females of upto 45 years age with more than three children.
Gallstone disease; Cholelithiasis; Serum lipids; Lipid profile; Cholesterol; Triglycerides; Free cholesterol
Application of FTIR and NIR Spectroscopy Coupled with Chemometrics for Determination of Monosodium Glutamate Level in Balado Seasoning
Balado seasoning is a spicy powder containing chili, spices and monosodium glutamate (MSG). MSG is a natural monosodium salt in the form of L-glutamic acid, used as a savory taste in food. This study aims to determine MSG in Balado seasoning using near-infrared (NIR) and Fourier transform infrared (FTIR) spectroscopy methods combined with hemometrics. The comparison method used was the thin layer chromatography (TLC)-Densitometry method. Support Vector Regression (SVR), Principal Component Regression (PCR) and Partial Least Square (PLS) were used to form a calibration model. Then the selected calibration model was validated by the leave one out cross validation (LOOCV) and external validation methods. Based on the research result, the PLS model is the selected calibration model with both the NIR and FTIR methods which gives the best results with an R2 value > 0.91. The results of the LOOCV validation have met the parameter values of R2 > 0.91, and the external validation result using the NIR and FTIR methods yielded R2 values of 0.999 and 0.997 and RMSEP value of 0.093 and 0.284, respectively. The concentration of MSG in commercial samples obtained by TLC Densitometry as a reference method were 1.314%, 1.449%, 5.836%, and 9.672%. The results of the analysis of MSG concentration as measured by the NIR and FTIR spectroscopy compared to TLC Densitometry did not give a significant difference.
Monosodium glutamate, NIR spectroscopy, FTIR spectroscopy, Chemometrics, Balado seasoning, TLC Densitometry
Evaluation of Complexation Behavior of Calix[4]arene Derivative
In this article we have explored the solvatochromic behavior including solvent selection, time study and complexation ability of 5,11,17,23-Tetrakis(N-piperidinomethyl)-25,26,27,28-tetrahydroxycalix[4]arene (3). The complexation behavior of 3 toward the selected transition metals has been explored through FT-IR, UV-visible and fluorescence spectroscopic techniques. It has been found that the ligand 3 has remarkable complexation ability for all selected transition metal (Cd2+, Cu2+, Ni2+, Co2+, Pb2+, Hg2+) ions used in the experiment with exceptionally high affinity for Hg2+ ions. Besides this, by applying method of continuous variation, i.e. Job's method; the stoichiometric ratio for the complexation between 3 and Hg2+ ion in acetonitrile has been determined, which indicates that 3 forms a 1:1 metal:ligand complex. The strong complexation behavior of 3 for Hg2+ ions was also confirmed by FT-IR and fluorescence spectroscopy. Consequently, it has been deduced that 3 is a versatile compound and can be used in diverse fields such as analytical/environmental chemistry and sensor technology.
Calixarene; Transition metals; Complexation; Liquid-Liquid Extraction; Jobs plot
Characterization of Humic Acid from the River Bottom Sediments of Burigonga: Complexation Studies of Metals with Humic Acid
In order to characterize and study of the complexation of humic acid with metal ions, sediment samples were collected from five different places in the Buriganga River. The Humic Acids were extracted with the standard procedure provided by the International Humic Substance Society (IHSS). The extracted Humic Acids were characterized with FTIR, EDX and CHNS analyzer and a comparison between the standard and extracted HA was carried out. High C/N ratios (71.48-87.36) are observed in the CHNS analysis. A complexation study of the Humic Acid with iron (III) and cadmium (II) was also carried out using EDX, UV-Visible spectrophotometer and AAS techniques. The coagulation behavior was observed with Jar test. From the study, it was found that iron and cadmium could make a complex at pH 6.0 which was confirmed by EDX (Electron Dispersive x-ray)
Humic acid; Iron; Cadmium; Complex; Buriganga river
Variation in Fatty Acids Composition Including Trans Fat in Different Brands of Potato Chips by GC-MS
Twelve different brands of potato chips were analyzed for their fatty acid compositions with eminence on trans fatty acid (TFA) using GC-MS. Results of the present study showed that the dominant fatty acids were saturated fatty acids. Among the saturated fatty acids, palmitic acid (23.9142.64 %) was found in greater amount in all analyzed chips samples. The amount of TFAs determined was ranged between (4.9114.13 %). Although there was significant variation in the fatty acid profile of all analyzed chips samples but high amount of palmitic acid and trans fat was commonly observed. The results of present study clearly indicated fat used in the manufacturing of chips was partially hydrogenated and palm oil had major contribution. The high level of trans as well as saturated fat is startling issue for the health of consumers.
Chips; Fatty acid profile; trans fatty acids; Chromatographic technique
Removal of Arsenic from Groundwater with Low Cost Multilayer Media
A simple, low cost arsenic removal system was developed to treat arsenic contaminated ground water containing 425 ± 4.2 µg/L arsenic. The system decontaminates arsenic from water by sorption through fine particles of waste materials (Coconut husks ash, Refused brick dust, Stone dust and Waste newspaper) of multilayer. The treatment efficiency of the process was investigated under various operating conditions that might affect the sorption/ desorption of arsenic. Sorption column method shows the optimum removal of As(III) under the following conditions: initial As concentration (100 µg/L), sorbent amount (4.0 g for brick dust, 3.0 g for stone dust, 3.0 g for Coconut husk-s ash and 0.3 g for waste newspaper), particle size (<355 µm), treatment flow rate (1.4 mL/min), optimum volume (100 mL) and pH (5.0). Desorption efficiencies with 2M of KOH after the treatment of groundwater were observed in the range of 78 ± 1.2% - 82 ± 1.4%. Average arsenic concentration of treated sample water was 8.30 ± 0.4 µg/L which is below the WHO guideline value for Bangladesh. Different techniques were used to measure thirteen metals, four anions with pH, conductivity, and temperature to understand the status of other species before and after treatment. The average concentrations of other inorganic constituents of health concern (Cu, Mn, Pb, Cr and Fe) in treated water were below WHO guideline value for drinking water. The present study showed a new method for removal of as from ground water
Arsenic; Removal; Sorption; Low cost; Multilayer
Sequential Microwave-Assisted Extraction of Oil from Layer Poultry Feeds and GC-MS Quantification of the Fatty Acids
The present study reports the effect of sequential microwave-assisted extraction (SeMAE) on fatty acids composition (FAC) of layer poultry feed oil as compared to conventional Soxhlet extraction (SE) method. The FAC of extracted oil was determined by gas chromatography-mass spectrometry (GC-MS). There was no significant difference found in the amount of total extracted oil and FAC by SeMAE and SE. However, slightly greater content of trans fat in the samples revealed that SE lead to the formation of a little higher level of trans fat as compare to SeMAE. Therefore, the SeMAE could be used as a remarkable substitute to conventional SE for extraction of oil from the poultry feeds due to its faster speed, lesser solvent consumption, more environmental friendly.
Layer poultry feed oil; Sequential microwave assisted extraction; Soxhlet extraction; Fatty acid composition; trans Fat.
Ethanol Production Kinetics by a Thermo-Tolerant Mutant of Saccharomyces Cerevisiae from Starch Industry Waste (Hydrol)
A thermo-tolerant and deoxyglucose-resistant mutant of Saccharomyces cerevisiae was developed and employed to convert them to fuel ethanol in a 150 litre fermenter. Maximum ethanol production was achieved when fermentation of dextrozyme- treated hydrol was carried out for about 36 hours under optimized fermenting conditions. The maximum specific ethanol production rate (qP), and overall ethanol yield (YP/S) were found to be 2.82 g L-1 h-1 and 0.49 g/g respectively. Determination of activation energy for cell growth (Ea= 20.8 kJ/mol) and death (Ed = 19.1 kJ/mol) and product formation and inactivation (EP=35.8 kJ/mol and Edp = 33.5 kJ/mol) revealed the thermo-stability of the organism for up to 47°C
Corn steep liquor; Hydrol; Temperature; Specific productivity; Product yield
Photoelectrochemical Sensors for the Rapid Detection of DNA Damage Induced by Some Nanoparticles
Photoelectrochemcal sensors were developed for the rapid detection of oxidative DNA damage induced by titanium dioxide and polystyrene nanoparticles. Each sensor is a multilayer film prepared on a tin oxide nanoparticle electrode using layer- by-layer self assembly and is composed of separate layer of a photoelectrochemical indicator, DNA. The organic compound and heavy metals represent genotoxic chemicals leading two major damaging mechanisms, DNA adduct formation and DNA oxidation. The DNA damage is detected by monitoring the change of photocurrent of the indicator. In one sensor configuration, a DNA intercalator, Ru(bpy)2 (dppz)2+[bpy=2, 2′ -bipyridine, dppz=dipyrido( 3, 2-a: 2′ 3′-c) phenazine], was employed as the photoelectrochemical indicator. The damaged DNA on the sensor bound lesser Ru(bpy)2 (dppz)2+ than the intact DNA, resulting in a drop in photocurrent. In another configuration, ruthenium tris(bipyridine) was used as the indicator and was immobilized on the electrode underneath the DNA layer. After oxidative damage, the DNA bases became more accessible to photoelectrochemical oxidation than the intact DNA, producing a rise in photocurrent. Both sensors displayed substantial photocurrent change after incubation in titanium dioxide / polystyrene solution in a time  dependent manner. According to the data, damage of the DNA film was completed in 1h in titanium dioxide / polystyrene solution. In addition, the titanium dioxide induced much more sever damage than polysterene. The results were verified independently by gel electrophoresis and UV-Vis absorbance experiments. The photoelectrochemical reaction can be employed as a new and inexpensive screening tool for the rapid assessment of the genotoxicity of existing and new chemicals.
Photoelectrochemical sensors; DNA damage; Nanoparticles
Spectrophotometric Assay of Phenylephrine Hydrochloride Using 4-Aminoantipyrine and Copper (II)
A new spectrophotometric method is proposed for determination of phenylephrine hydrochloride. The method is based on the coupling of 4-aminoantipyrine (4-AAP) with phenylephrine hydrochloride (PEH) to give a new ligand that reacts with copper (II) in the presence of sodium tetraborate buffer solution of pH 9.00 at 50 °C to give an intense red colored chelate having maximum absorption at 480 nm. The optimization of the experimental conditions is described. The method has been used for the determination of 2.050.0 ìg/ml of PEH. The molar absorptivity is 5.34×103 L.mol.-1cm.-1 and the accuracy of the method is achieved by the value of average recovery (101.28 %) and the precision is supported by relative standard deviation (RSD=1.25 %) values. The results of the method was compared with those of the standard method. The interference of excipients was studied. The mechanism of the chemical reaction has been proposed. The proposed method was successfully applied for the determination of the PEH in pharmaceutical syrup formulations.
Phenylephrine; 4-Aminoantipyrine; Copper(II); Spectrophotometry.
Analysis of Protein by Spectrophotometric and Computer Colour Based Intensity Method from Stem of Pea (Pisum sativum) at Different Stages
In this study proteins were analyzed from pea plants at three different growth stages of stem by spectrophotometric i.e Lowry and Bradford quantitative methods and computer colour intensity based method. Though Spectrophotometric methods are regarded as classical methods, we report an alternate computer based method which gave comparable results. Computer software was developed the for protein analysis which is easier, time and money saving method as compared to the classical methods.
Protein, Spectrophotometer, Computer software, Dye and colour intensity