Quality Control of Some Water, Food, and

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• Quality Control of Some Water, Food, and
• Drug Samples in Erbil City, Iraq
• Prof. Dr. Nabil A. Fakhre
• Dept. of Chemistry, College of Education/
  Scientific Depts., Univ. of Salahalddin, Erbil,
  IRAQ
• nabil_fakhri_at_yahoo.com

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• Qualitycontrol (QC) is a procedure or set of
  procedures intended to ensure that a manufactured
  product or performed service adheres to a defined
  set of quality criteria or meets the requirements
  of the client or
• customer.
• This global quality management system provides
  the basis for analyzing customer requirements,
  defining theprocesses that contribute to the
  achievement of a productor service that is
  acceptable to the customer, and provisions for
  keeping these processes in control.
• QC activities include general methods such as
  accuracy checks on data acquisition and
  calculations and the use of approved standardized
  procedures for emission calculations,
  measurements, estimating uncertainties, archiving
  information and reporting.
• Higher tier QC activities include technical
  reviews of source categories, activity and
  emission factor data, and methods.

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• SEMI-AUTOMATED DETERMINATION OF NITARATE IN TAP
  WATER SAMPLES USING DIZOTIZATION- COUPLING
  REACTION
• Nabil A. Fakhre, and Hemen A. Kadir
• Nitrate is an important intermediate in the
  biogeochemical cycling of nitrogen in natural
  water. Because of the relative stability of the
  nitrate ion, most nitrogenous materials in
  environmental media tend to be converted to
  nitrate. Therefore, all sources of nitrogen
  (including organic nitrogen, ammonia and
  fertilizers) should be considered as potential
  sources of nitrate. Nitrate is relatively
  non-toxic, and it can be converted readily by
  bacteria to nitrite, which is also one of the
  pollutants in the atmosphere and natural water.
  Nitrate, converted to nitrite, may reacted with
  amines (proteins found in some foods,
  medications, and water) to produce nitrosamines,
  which have been found to be carcinogenic in
  animals. Some of types of cancer linked to this
  reaction.
• The maximum contaminated level for nitrate in
  drinking water is 45 ppm, and the value of total
  nitrogen at the outlet of wastewater plant or in
  rivers and lakes should be below 18 ppm, which
  equivalent to about 59 ppm of nitrite and 79.7
  ppm nitrate.
• Semi- automated method has been investigated for
  the determination of nitrate depending upon the
  reduction of nitrate to nitrite using a
  mini-column of amalgamated cadmium redactor. The
  produced nitrite was reacted with N,
  N-dimethyl-p-phenylenediamine dihydrochloride
  (NDMPDAH), to produce a water soluble, colorless
  diazonium ion, which subsequently coupled with
  resorcinol to form an azo dye in the alkali
  medium to be detected in a spectrophotometer with
  a flow cell of 30 ul. Nitrate was determined in
  the concentration range (0.3- 6.0) ppm with
  detection limit 0.15 ppm and sampling rate of 60
  samples/h.
• The method is with acceptable precision and
  accuracy depending upon the values of relative
  standard deviation and relative error percentage.
  The effect of 35 cations and anions on the
  determination of nitrate was studied. To
  eliminate the influence of some cations two
  methods have been used column of cationic
  exchanger and EDTA solution.
• The method was applied successfully for
  determination of nitrate in various wastewater
  samples in different locations in Erbil City
  after the removal of turbidity, oil and grease.
  The results were compared to those obtained with
  standard NEDA method.
•  

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• Extraction-Spectrophotometric Determination of
  Nitrate in Polluted Water and Soil Samples using
  Diazo-Coupling Reaction
  
  
• Chinar M. Rasheed and Nabil A. Fakhre
  
  
• Department of Chemistry, College of Education,
  University of Salahalddin, Erbil, Iraq
•  
• Abstract
• A simple and sensitive spectrophotometric
  method was described for the determination of
  nitrate. The method is based on the reaction of
  nitrite with 3-amino-5-methyl isoxazole to form a
  diazonium ion, which is coupled with resorcinol
  in an alkaline medium to form the azo dye, with a
  maximum absorption at 354 nm. Nitrate is
  determined by its reduction to nitrite using
  amalgamated cadmium column. Beers law is obeyed
  over the range of 0.04-6 ?g/ml, with a detection
  limit of 0.02?g/ml. The molar absorptivity,
  Sandell index are 2.482 x 104 L/mol.Cm and
  0.00249 ?g/ml respectively . The effect of 35
  cations and anions were studied. The method was
  applied for determination of nitrate in polluted
  water and soil samples, the results were
  compaired with the standard method, NEDA. The
  prepared azo dye was extracted into 11 (v/v)
  mixture of isoamyl alcohol-isobutyl methyl
  ketone. Nitrate was determined over the range of
  0.005-2 ?g/ml with a detection limit of 0.003
  ?g/ml and molar absorptivity 6.486 x 104 L/mol.
  cm.

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• Spectrophotometric Determination of Nitrite in
  Curing Meat Samples
•  
• Nabil A. Fakhre and Hemn A. Qader
•  
• Nitrite ion is an important intermediate
  in biological nitrogen cycle and is present in
  soils and surface waters. Nitrite is also a
  versatile chemical agent, which has found
  numerous applications ranging from dye
  manufacture to food preservation. Alkali nitrites
  and nitrates, along with sodium chloride have
  long been used in the curing of meat products to
  prevent bacterial spoilage and to enhance the
  flavor, color and texture of these food products.
  Nitrite oxidizes hemoglobin to methemoglobin,
  which is unable to transport oxygen, and nitrites
  react with amines and amides to form
  nitrosamines, which are potent carcinogens.
  Current legislation (EU Directive 95/2) suggests
  maximum amounts to be added at the beginning of
  processing in various meat products and imposes a
  maximum residue of 50 µg/ml nitrites and 250
  µg/ml nitrates in cured meat products that have
  not been thermally treated.
• The nitrite content in meat products has been
  regulated and the majority of the analytical
  methods recommended by the legislations of
  different countries to determine its content are
  based on the Saltzman modification of the
  classical Griees method. Many methods have been
  reported for the spectrophotometric determination
  of nitrite .
• In the present work, a simple procedure for the
  spectrophotometric determination of nitrite is
  described. The method is based on the reaction of
  acidified 2-aminobenzoimidazole as the
  diazotizing agent with nitrite to produce water
  solublediazoniumion, which subsequently coupled
  with orcinol to give azo dye having maximum
  absorption at305nm. The method has been
  successfully applied to the determination of
  nitrite in curing meat samples.
•  

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• DETERMINATION of ACRYLAMIDE in POTATO CHIPS
  SAMPLES USING DIFFERENT ANALYTICAL TECHNIQUES
•  
• Nabil A. Fakhre and Bnar M. Ibrahim
• Chemistry Department, College of Education
  /Scientific Departments,University of Salahaddin,
  Erbil / Kurdistan Region, Iraq
• havras_at_yahoo.com
•  
• Acrylamide is formed in some foods cooked
  at high temperature (120-170ºC) by the reaction
  of the amino acid asparagines with a reducing
  sugar such as glucose. Acrylamide is genotoxic
  and carcinogenic in studies in animals. It causes
  increased tumour incidence at a variety of sites.
  The international agency on research on cancer
  has classified acrylamide as probably
  carcinogenic to humans. Two sensitive and fast
  batch and flow-injection spectrophotometric
  methods for the determination of acrylamide are
  proposed. The methods were based on
  oxidation-reduction reaction of acrylamide with
  potassium permanganate. The calibration graphs
  are linear over the ranges 1.08.0 and
  2.0-13µg/ml of acrylamide, with detection limits
  of 0.6 and 1.0µg/ml, respectively. The methods
  are applied to the routine analysis of acrylamide
  in potato chips samples. It confirms that the
  analytical procedure employed for the analysis is
  suitable and reliable for its intended use.
  Acrylamide was also determined in the presence of
  glucose and asparagines. Reduction of some
  cationic interference was carried out in the
  batch and flow injection analysis using cationic
  exchanger of hydrogen form with 2.5 mm internal
  diameter, 15-cm length of packing and flow rate
  0.5 ml/min. The proposed first and second
  derivative methods for determination of
  acrylamide, are simple, rapid (as it only
  requires measurements of nD values at a single
  wavelength). They were used for identification of
  the acrylamide depending upon characteristic
  peaks at certain wavelengths or ranges. The first
  and second derivative spectra of the mentioned
  compound have been used for determination of the
  compounds at different ranges of concentration
  depending upon the measurements of the heights of
  the peak to the baseline at certain wavelengths.
  HPLC was used as a standard method for
  qualification and quatitation of acryl amide in
  different potato chips samples, and the results
  obtained were agreed with those of the proposed
  methods.

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• Online separation and preconcentration for
  histamine determination
• in fish meal using cation exchanger resin
•  Nabil A. Fakhre and Mohammad S. Abdulla
•   Biogenic amines are a group of biologically
  active organic compounds normally produced by
  decarboxylation of free amino acids. Biogenic
  amines are present in a variety of foods and have
  been widely documented as occurring in fish and
  fish products, meat, wine, cheese and fermented
  foods. The presence of biogenic amines in these
  foods is an indication of food spoilage which is
  dependent upon the availability of free amino.
• Histamine, which is the most important biogenic
  amine, can cause poisoning as a result of the
  ingestion of food containing high levels of this
  amine.
• To a series of 25 ml volumetric flasks, 4.0 ml
  of 0.2 p-toluidine (prepared in 0.5M HCl), 0.5
  ml of 0.5 sodium nitrite, 12.5 to 175 µg of
  histamine and 2.0 ml of 1M KOH were added. The
  solution completed to mark with ethanol after two
  minutes. Absorbance measurements were carried out
  against reagent blank. Fig. 2-2 shows FI
  manifold used for histamine determination. A
  multi channel peristaltic pump was used for
  propelling p-toluidine (0.5 in 1M hydrochloric
  acid) solution, 0.5 sodium nitrite solution and
  1M potassium hydroxide solution, with flow rates
  0.9, 0.8 and 0.4 ml/min for solutions
  respectively. A 175 µl of histamine sample was
  injected through the injection valve. Three
  reaction coils were used in the system with
  lengths 5cm (RC1), 40cm (RC2) and 40cm (RC3). The
  merged streams were passed through a quartz flow
  cell (30 µl, 10 mm path length) in a
  spectrophotometer.

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• FlOW-INJECTION SPECTROPHOTOMETRIC DETERMINATION
  OF CHLOROGENIC ACID IN SOME NATURAL SAMPLES
• Nabil, Adil Fakhre and Rizgar Mohamad Hassan
•  
• Polyphenols, are a group of chemical substances
  present in plants which play an important role
  during enzymatic browning. They are responsible
  for the color of many plants, such as apples
  part of the taste and flavor of beverages (apple
  juice, tea). Chlorogenic acid (CGA) is a major
  phenolic natural product isolated from the leaves
  and fruits of dicotyledonous plants, including
  the coffee beans which typically contain 5-8 of
  CGA. Biologically, it is an important polyphenol
  it is found widely in plants, black teas, soya
  beans, wheat, apple juice, tobacco, some
  traditional Chinese medicines, beers, wines,
  Chinese herbs2 and accounting for gt 75 of the
  total phenolic acids content extracted from the
  eggplant sample, also the presence of CGA in
  sunflower seeds is well-known.
• CGA not only has the function of antioxidation,
  inhibiting hypertension and stimulating the
  flowering of plants, but also affects the
  activity of trypsin, amylase and other enzymes.
  CGA is the main component producing the bitter
  taste in crude coffee and thus deliberative
  elimination of CGA into the instant coffee has
  been adopted extensively to improve the taste of
  various kinds of coffees. The contents of CGA in
  different areas and in various foods are also
  quite different. Therefore, it is very important
  to establish some quantitative methods to monitor
  the concentration of CGA in all kinds of real
  samples.
• A flow-injection spectrophotometric system was
  applied for determination of chlorogenic acid
  using 3-amino-5-methylisoxazole as diazotizing
  agent in the linear range of 1.0-50.0 ?g/ml, with
  the sample volume of 175 µl and the detection
  limit of 0.30 ?g/ml. The rate of sampling was 60
  samples/h, with the RSD and Error of 2.254 and
  3.4966, respectively. The influences of
  seventeen phenolic compounds (as interferences)
  such as dopamine, tyrosine, catechol, tannin, 2,
  4-dihydroxybenzoic acid, caffeic acid and
  p-cresol on determination of chlorogenic acid
  were studied. An ultrasonic technique was used
  for extracting chlorogenic acid in the samples by
  using 80 (v/v) methanol aqueous solution. The
  proposed method was successfully applied for the
  determination of chlorogenic acid content in
  various natural samples such as grape, tobacco
  and black tea.

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• Studies on Physico - Chemical Characteristics of
  Some Edible Oils
• and
• Authentication of Triacylglycerols using HPLC
• Nabil A. Fakhre and Hemen K. Kadir
• The aim of the study
• It is intended to study the properties of some of
  edible oil samples through the phsico - chemical
  tests like (refractive index, specific gravity,
  viscosity, iodine value, peroxide value,
  percentage of free fatty acid and pH value). The
  study aims to shed more light on the oil acidity
  and composition of saturated and unsaturated
  fatty acids.
• The adulteration was the second aim of the
  present study using (RP-HPLC/RI detector) to
  confirm authenticity of triacylglycerols and to
  identify the composition of blends of some edible
  vegetable oils.

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• FLOW-INJECTION AND STOPPED FLOW
  SPECTROPHOTOMETRIC DETERMINATION OF DOPAMINE
  HYDROCHLORIDE IN PHARMACEUTICAL PREPARATIONS
• Nabil A. Fakhre, and Mohamad S. Abdullah
• Dept. of Chemistry, College of Science Education,
  Univ. of Salahaddin, Erbil, IRAQ.
• havras_at_yahoo.com
• Key words Flow-injection, Stopped flow,
  Spectrophotometric determination, Dopamine.
• The catecholamines participate in the regulation
  of a wide variety of physiological function in
  humans. In principle they control cardiac output
  and apportion blood flow. Dopamine is one of most
  significant catecholamines. It is naturally
  occurring amine used for treatment of acute
  congestive failure and renal failure. Dopamine
  hydrochloride is determined by flow injection and
  stopped-flow. The assay depends on the
  nitrosation of the aromatic ring followed by
  forming a stable colored compound in alkali
  medium. The reaction has a maximum absorption at
  377nm. The method obeyed Beer s law in the range
  40-160µg/ml. The number of sample throughput is
  35s/hour with injected sample 200µl. To increase
  the sensitivity of the method stopping flow of
  the reaction zone in the flow cell at a regulated
  time after the injection of sample was made. The
  optimum time of stopping was 60 sec. The method
  obeyed Beer s law in the range 15-120 µg/ml.
  Both methods were applied for determination of
  dopamine hydrochloride in pharmaceutical
  preparation with recoveries 95.0-97.0.

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• Flow injection Spectrophotometric Determination
  of Folic Acid in Some
• Pharmaceutical Preparations using
  Diazotizing-Coupling Method
• Nabil Adil Fakhre and Mohammad Salim Abdullah
• Folic acid (FA) is extremely important vitamin
  that occurs naturally in foods. It is essential
  for human. Folacin is a generic name covering FA
  and related compounds having the same biochemical
  activities of FA. Folic acid and folate (the
  anion form) are forms of water soluble B-vitamins
  ( Champe and Harvey,1994). It plays a key role in
  one-carbon metabolism, and is essential for the
  biosynthesis of the purines and pyrimidines.
  Folic acid deficiency is probably the most common
  vitamin in USA, particularly among pregnant women
  and alcoholism ( Marks et.al,1996) . Folic acid
  helps form building blocks of DNA, the body
  genetic information, and building blocks of
  RNA, needed for protein synthesis in all cells.
  
• The present study describes a simple, rapid and
  sensitive method for the determination of folic
  acid at 435nm. Folic acid was diazotizated with
  nitrous acid then coupled with sulphanilic acid.
  Nitrous acid (0.5 NaNO2 in 0.5M HCl), 0.1
  sulphanilic acid and 0.25M sodium hydroxide
  solutions were propelled at flow rates 0.6ml/min.
  Folic acid solution (10µg/ml) was injected with
  sample volume 125µl to react with the nitrous
  acid solution in a reaction coil of 10-cm. The
  proposed flow system method was linear in the
  range 6.0 to 25.0 µg/ml. The precision and
  accuracy of the methods were checked. The effects
  of foreign species were tested. The proposed
  method was successfully applied to the
  determination of folic acid in commercial folic
  acid tablets. The results are compared with that
  of standard method (HPLC).

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• Determination of Gasoline and Kerosene in a
  Mixture Using Peak-to -Peak Derivative
  Spectroscopic Method
• Nabil A. Fakhre
• Although UV-visible spectra do not enable
  absolute identification of an unknown substance,
  they frequently are used to confirm identity
  through comparison of the measured spectrum with
  a reference spectrum. Typical multispectral
  analysis methods treat each spectral band as an
  independent variable, a reasonable assumption for
  multispectral data but not really appropriate for
  hyperspectral data. In spectroscopy, particularly
  in infra-red, UV and visible absorption,
  fluorescence, and reflectance spectrophotometry,
  differentiation of spectra is a widely used
  technique, referred to as derivative
  spectroscopy. Derivative spectroscopy has the
  potential of greatly increasing the application
  of UV-visible spectroscopy. Derivative methods
  have been used in analytical spectroscopy for
  three main purposes, spectral discrimination,
  spectral resolution enhancements, and
  quantitative analysis. Therefore, a simple and
  rapid method is described for the simultaneous
  quantitative analysis of gasoline and kerosene in
  a mixture using first, second, third and fourth
  derivative spectroscopy. Peak-to-peak heights
  were used to find various concentration ranges of
  gasoline and kerosene. First derivative spectra
  were used for determination of 10-60 and 40-80
  Gasoline and 40-90 and 20-60 kerosene. Whereas
  second and third derivative spectra have been
  used for determination of 40-80 gasoline and
  20-60 kerosene. Fourth derivative spectra were
  used for determination of 20-80 gasoline and
  kerosene.

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Thank you for your attention