Determination pharmaceutical

Hancock, B. C. and S. L. Shamblin. 2001. Molecular mobility of amorphous pharmaceuticals determined using differential scanning calorimefrlsrermochim ActS80 95-107. 

Pharmaceuticals. Determination of drug candidate/metabolite structure in discovery and development studies end product and intermediate purification... 

Berberine,acrino1 Quaternary alkyl amines Analysis pharmaceuticals Determination by using UV-absor-bing counter-ions(Fig,15.2)... 

M. A. Koupparis, P. Anagnostopoulou, and H. V. Malmstadt, Automated Flow-Injection Pseudotitration of Strong and Weak Acids, Ascorbic Acid and Calcium, and Catalytic Psudotitrations of Aminopolycarboxylic Acids bu Use of a Microcomputer-Controlled Analyser. Talanta, 32 (1985) 411. A. Rios, M. D. Luque de Castro, and M. Valc rcel, Flow Injection Analysis A New Approach to Pharmaceutical Determinations. J. Pharm. Biomed. Anal., 3 (1985) 105. 

MAJOR USES Used as a solvent in glues, varnishes, cements and inks used in the industries of dry cleaners, pesticides, thermometers, fuel, alcohol, pharmaceuticals determination of refractive index of minerals. 

Although kinetic methods of analysis are of special significance to clinical and pharmaceutical analysis in relation to enzymatic methods, they are equally applicable to nonenzymatic processes. Table 7 shows the most salient contributions reported in this respect over the past few years. Most of the clinical determinations shown have been performed on blood and/or urine samples and have involved inorganic or organic ions in similar proportions. On the other hand, pharmaceutical determinations have chiefly been concerned with organic substances. The Sandell-Kolthoff reaction has by far been the most commonly employed for the analysis of biological samples, so much... 

Chen, I, Korfmacher, W.A., Hsieh, Y. (2005) Chiral liquid chromatography-tandem mass spectrometric methods for stereoisomeric pharmaceutical determinations. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 820,1-8. 

Hancock BC, Dalton CR (1999) The effect of temperature on water vapor sorption by some amorphous pharmaceutical sugars. Pharma Dev Technol 4 125-131 Hancock BC, Shamblin SL (2001) Molecular mobility of amorphous pharmaceuticals determined using differential scanning calorimetry. Thermochim Acta 380 95-107 Hancock B, Dalton C, Pikal M, Shamblin S (1998) A pragmatic test of a simple calorimetric method for determining the fragility of some amorphous pharmaceutical materials. Pharm Res 15 762-767... 

Some studies have reported the applications of CCC into pharmaceutical determinations. 

TEOS-Doped Nano-Optical Sensor for Pharmaceutical Determinations... 

Xiang, D., Konigsberger, M., Wabuyele, B., Homung, K. and Cheney, J. Development of robust quantitative methods by near-infrared spectroscopy for rapid pharmaceutical determination of content uniformity in complex tablet matrix. Analyst 134 1405-1415, 2009. 

A challenging task in material science as well as in pharmaceutical research is to custom tailor a compound s properties. George S. Hammond stated that the most fundamental and lasting objective of synthesis is not production of new compounds, but production of properties (Norris Award Lecture, 1968). The molecular structure of an organic or inorganic compound determines its properties. Nevertheless, methods for the direct prediction of a compound s properties based on its molecular structure are usually not available (Figure 8-1). Therefore, the establishment of Quantitative Structure-Property Relationships (QSPRs) and Quantitative Structure-Activity Relationships (QSARs) uses an indirect approach in order to tackle this problem. In the first step, numerical descriptors encoding information about the molecular structure are calculated for a set of compounds. Secondly, statistical and artificial neural network models are used to predict the property or activity of interest based on these descriptors or a suitable subset. 

Perhaps the most common type of problem encountered in the analytical lab is a quantitative analysis. Examples of typical quantitative analyses include the elemental analysis of a newly synthesized compound, measuring the concentration of glucose in blood, or determining the difference between the bulk and surface concentrations of Cr in steel. Much of the analytical work in clinical, pharmaceutical, environmental, and industrial labs involves developing new methods for determining the concentration of targeted species in complex samples. Most of the examples in this text come from the area of quantitative analysis. 

Many pharmaceutical compounds are weak acids or bases that can be analyzed by an aqueous or nonaqueous acid-base titration examples include salicylic acid, phenobarbital, caffeine, and sulfanilamide. Amino acids and proteins can be analyzed in glacial acetic acid, using HCIO4 as the titrant. For example, a procedure for determining the amount of nutritionally available protein has been developed that is based on an acid-base titration of lysine residues. ... 

The purity of a pharmaceutical preparation of sulfanilamide, C6H4N2O2S, can be determined by oxidizing the sulfur to SO2 and bubbling the SO2 through H2O2 to produce H2SO4. The acid is then titrated with a standard solution of NaOH to the bromothymol blue end point, where both of sulfuric acid s acidic protons have been neutralized. Calculate the purity of the preparation, given that a 0.5136-g sample required 48.13 mL of 0.1251 M NaOH. 

Industrial Analysis UV/Vis molecular absorption is used for the analysis of a diverse array of industrial samples, including pharmaceuticals, food, paint, glass, and metals. In many cases the methods are similar to those described in Tables 10.6 and 10.7. For example, the iron content of food can be determined by bringing the iron into solution and analyzing using the o-phenanthroline method listed in Table 10.6. 

Many pharmaceutical compounds contain chromophores that make them suitable for analysis by UV/Vis absorption. Products that have been analyzed in this fashion include antibiotics, hormones, vitamins, and analgesics. One example of the use of UV absorption is in determining the purity of aspirin tablets, for which the active ingredient is acetylsalicylic acid. Salicylic acid, which is produced by the hydrolysis of acetylsalicylic acid, is an undesirable impurity in aspirin tablets, and should not be present at more than 0.01% w/w. Samples can be screened for unacceptable levels of salicylic acid by monitoring the absorbance at a wavelength of... 

Description of Method. The amount of chlorpromazine in a pharmaceutical formulation is determined voltammetrically at a graphite working electrode in a nonstirred solution. Calibration is achieved using the method of standard additions. 

Vogt, C. Conradi, S. Rhode, E. Determination of Caffeine and Other Purine Compounds in Pood and Pharmaceuticals by Micellar Electrokinetic Chromatography, /. Chem. Educ. 1997, 74, 1126-1130. 

Let s use a simple example to develop the rationale behind a one-way ANOVA calculation. The data in Table 14.7 show the results obtained by several analysts in determining the purity of a single pharmaceutical preparation of sulfanilamide. Each column in this table lists the results obtained by an individual analyst. For convenience, entries in the table are represented by the symbol where i identifies the analyst and j indicates the replicate number thus 3 5 is the fifth replicate for the third analyst (and is equal to 94.24%). The variability in the results shown in Table 14.7 arises from two sources indeterminate errors associated with the analytical procedure that are experienced equally by all analysts, and systematic or determinate errors introduced by the analysts. 

Table 14.7 shows the results obtained by four analysts determining the purity of a pharmaceutical preparation of sulfanilamide. Determine if the difference in their results is significant at a = 0.05. If such a difference exists, estimate values... 

The value of many chemical products, from pesticides to pharmaceuticals to high performance polymers, is based on unique properties of a particular isomer from which the product is ultimately derived. Eor example, trisubstituted aromatics may have as many as 10 possible geometric isomers whose ratio ia the mixture is determined by equiHbrium. Often the purity requirement for the desired product iacludes an upper limit on the content of one or more of the other isomers. This separation problem is a compHcated one, but one ia which adsorptive separation processes offer the greatest chances for success. 

Miscellaneous Pharmaceutical Processes. Solvent extraction is used for the preparation of many products that ate either isolated from naturally occurring materials or purified during synthesis. Among these are sulfa dmgs, methaqualone [72-44-6] phenobarbital [50-06-6] antihistamines, cortisone [53-06-5] estrogens and other hormones (qv), and reserpine [50-55-5] and alkaloids (qv). Common solvents for these appHcations are chloroform, isoamyl alcohol, diethyl ether, and methylene chloride. Distribution coefficient data for dmg species are important for the design of solvent extraction procedures. These can be determined with a laboratory continuous extraction system (AKUEVE) (244). 

The fermentation-derived food-grade product is sold in 50, 80, and 88% concentrations the other grades are available in 50 and 88% concentrations. The food-grade product meets the Vood Chemicals Codex III and the pharmaceutical grade meets the FCC and the United States Pharmacopoeia XK specifications (7). Other lactic acid derivatives such as salts and esters are also available in weU-estabhshed product specifications. Standard analytical methods such as titration and Hquid chromatography can be used to determine lactic acid, and other gravimetric and specific tests are used to detect impurities for the product specifications. A standard titration method neutralizes the acid with sodium hydroxide and then back-titrates the acid. An older standard quantitative method for determination of lactic acid was based on oxidation by potassium permanganate to acetaldehyde, which is absorbed in sodium bisulfite and titrated iodometricaHy. 

Methylene iodide [75-11-6], CH2I2, also known as diio dome thane, mol wt 267.87, 94.76% I, mp 6.0°C, and bp 181°C, is a very heavy colorless Hquid. It has a density of 3.325 g/mL at 20°C and a refractive index of 1.7538 at 4°C. It darkens in contact with air, moisture, and light. Its solubiHty in water is 1.42 g/100 g H2O at 20°C it is soluble in alcohol, chloroform, ben2ene, and ether. Methylene iodide is prepared by reaction of sodium arsenite and iodoform with sodium hydroxide reaction of iodine, sodium ethoxide, and hydroiodic acid on iodoform the oxidation of iodoacetic acid with potassium persulfate and by reaction of potassium iodide and methylene chloride (124,125). Diiodoform is used for determining the density and refractive index of minerals. It is also used as a starting material in the manufacture of x-ray contrast media and other synthetic pharmaceuticals (qv). 

Other appHcations of firefly hioluminescence include measurement of the activity of bacteria in secondary sewage treatment activated sludge (296,297), detection of bacteria in clean rooms and operating rooms, measurement of bacteria in bottled foods, beverages (298), and pharmaceuticals (299), determination of the antimicrobial activity of potential dmgs (300), determination of the viabiHty of seeds (301), and measuring marine biomass concentrations as a function of ocean depth or geographical location (302). 

Although the techniques described have resulted in the determination of many protein stmctures, the number is only a small fraction of the available protein sequences. Theoretical methods aimed at predicting the 3-D stmcture of a protein from its sequence therefore form a very active area of research. This is important both to understanding proteins and to the practical appHcations in biotechnology and the pharmaceutical industries. 

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