quali/ quanti ppt

100問 • 1年前

問題一覧

-reveals the identity of the sample elements and compounds in the sample -presence or absence of components -e.g: USP sample test

qualitative analysis

-indicates the amount of each substance in the sample -exact amount or proportion of components expressed in 1% purity and compared to official compendia -e.g: gravimetric, volumetric, physichochemical and special methods of analysis.

quantitative analysis

*for crude drugs -proximate -ultimate *for chemical drugs -proximate -complete

based on extent

total of class of plant principles (group of compounds) *e.g: total alkaloidal compound in coffee beans

proximate

single chemical species (specific components) *eg: total caffaine content in coffee beans

ultimate

-selected or trace compounds

proximate partial

each constituent

complete

--chemical or general methods: titration, gravimetry --instrumental methods: UV-Vis, IR, MS, chromatography --special methods: ash content, water content, constants for fats and fixed oils

based on nature

what is used in in chemical methods for natural products

titration, gravimetry

what is used in instrumental method for natural products?

UV-Vis, IR, MS, chromatography

what special methods are used for natural products?

ash content, water content

-chemical compound reagents -physical boiling point, melting point, optical purity, refractive index *biological potency or effectivness of drugs: animal models; microbial assay- antibiotics

based on material

*AKA intermediate error -due to UNCONTROLLED variables -variations in a series of observations (by the same observer under identical condition) -AFFECT MEASURE PROPORTION

random error

-AKA determinate error >with definite value and identifiable cause >same magnitude or replicate measurements made the same way >CCAN LEAD TO BIAS ND AFFECT ACCURACY OF RESULTS *instrumental errors *method errors *personal errors

systematic error

*occurs occasionally; are often large, and may cause result to be either high or low *OFTEN A PRODUCT OF HUMAN ERROR

gross error

*CLOSENESS of an ACTUAL value to the THEORITICAL (true) value and is expressed by error - measures agreement between result and accepted value *absolute error *relative error

accuracy

-closeness of TWO OR MORE actual measurements obtained in exactly the same way -describes the REPRODUCIBILITY of measurement *overage deviation *standard deviation *coefficiennt of variation or range

precision

overage or arithmetic ____ -obtainedby dividing the sum of replicate measurements by the number of measurements in the set

mean

-middle result when replicate data are arranged in increasing or decreaing order -less affected by extreme values (outliers)

median

-AKA volumetric analysis +method in wwhich the volume of a solution of KNOWN concentration during anlysis is taken as the AMOUNT of ACTIVE constituent in the sample

titrimeric analysis

-AKA analyte/active constituents *sample being analyzed

titrand

reagents of known concentration -AKA volumetric/standard solution

titrant

compounds capabl of changing colors near the end

indicators

AKA stochiometric point -theoritical point at which equivalent amounts of the analyte and titrant have reached -N1V1=N2V2 or M1V1=M2V2 (molarity is used when the stochiometric point between titrant and titrand is 1:1)

eqivalence point

actual point aquivalent amounts of the analyte and titrand have reacted *point where a physical change occurthat is associated with the condition of chemmical equivalence

endpoint

-substance of HIGH DEGREE -serves as a REFERENCE MATERIAL (standard) in titrations -used in direct standardization purposes

primary standard

standard solutions whose purity has been determined by chemical analysis -used in INDIRECT standardization process

secondary standard

AKA: reaction capacity values * number of reacting entities per reagent

equivalence factor (F)

1 titrant

direct titrtion

2 titrants -AKA bak titration *1st VS added in EXCESS; 2nd VS used to titrate the excess (unreacted) 1st VS (bak titrant) indications: insoluble sample, volatile sample resection too slow, it does not give a sharp endpoint

residual titration

-for correction -to enhance the reliability of the endpoint

blank determination

*measurement of base by a standard acid indicators (aquaeous)- uses water as solvent SA+SB= phenolphthalein, methyl orange/red (non aquaeous)-non polar very week acid/base

acidemetry

measurement of an acid by a standard base

alkalimetry

*VS: KMNO4 *1st std: na2c2o4 *indicator: non (sef indicating) *endpoint: slight pink example assay -direct:h4o2 -indirect: malic acid contect of cherry juice -residual (oxalic acid-back titrant): kno4, nano2, kmno4

permanganoometry

assay for RA: I2+RA --2I-VS:I2 *first std: arsenic o3 *indicator: starch (appearance of blue) sample assay:: -direct: vit.C -residual: nahso3, methionine

iodimetry

assay for OA: rxn: 2I-+OA(sx)--I2 I2 +2S2O32- -- 2I-+s4o62- *VS: nas2o3 *1st std: k2cr2o2 *indicator: starch (disappearance of blue) example assay: -direct: cuso4, naocl -residual: phenol, resorcinol,thyroid hormones, ses2

iodometry

*VS:ce(so4)2 *1st std: as2o3, fe filling(old) *indicator: o-phennatrolin endpoint: red to blue example assay: -direct: feso4, feso4 tab, hydroquinone, menadione

cerimetry

*VS: EDTA *1st std: caco3 indicators: *eriochrome back T (EBT)-mg, zn *hydroxynahthol blue (hnb)- ca *dithiozone (dt)- al, bi example assay: -direct: zno, bi content of glycobiarsol (in all EDTA complexation reaction, ratio of EDTA to metal is 1:1 [EDTA]= molarity

complexation

determination of a metal in the presence of anothe metal masking agents: *triethanolamines: fe, mn, al *thioglycols: hg, cu, pb, bi **cyanide: cu, co, ni, zn *flourine: ca, mg, al

mmasking

volhard titration

residual

volhard VS

nh4scn

primary std used in volhard

agno3

indicator in volhard

ferric ammonium sulfate

endpoint in volhard

reddish brown

mohr titration

direct

primary std used in mohr

nacl

vs used in mohr

agno3

indicator used in mohr

k2cro4

endpoint in mohr

brick red ppt

fajans titration

direct

vs used in fajans

agno3

primary std used in fajans

dichloroflourecein, eosin y, tee (adsorption indicators)

en dpoint in fajans

green to pink (dcf)

a branch of science that studies the interaction between electromagnetic radiation and matter *principle: the intensity of radiant energy transmitted, reflcted, or emitted is related to the concentration of the cheical species that absorbs energy

spectroscopy

functional group that absorbs maximum radiation in the uv or visible regions

chromophore

fnctional group which does not give rise to a bsorption band by itself, but upon being attracted to a chromophore

auxochrome

- a form of energy that has both wave and particle properties -described by means of a classical sinusoidal wave model

electromagnetic radiation (emr)

point with the maximum upward displacement

crest

point with the maximum downward displacement

trough

the aximum height of a wave

amplitude

the disance between two identical adjacent point in a wave

wavelength

the numer of cycles per unit distance

wave number

the time required for one cycle to pass a fixed point in waves

period

the number of cycles which pass a fixed point in space per secnd

frequency

-since the speed of light in a vacuum is constant, there is an inverse relationship between wavelength and frequency *the higer the frequency, the shorter the wavelength *the longer the wavelength,, the lower the frequency

wave equation

*energy is directly prportinal to frequency *energy is inversely proportionl to wavelength e=hv

planck's equation

transmittance decrase exponentially as the concentration of the solution increases arithmethically

beer's

transmittance decreases exponentially as the thickess of the solution increases arithmethically

lambert's

-geenrates beam of radiation *continuum sources (ex: deuterium lamp, tungsten lamp,nernst glower) *line sources (ex; hollow cathode)

source of radiation

-isolates the restricted region of spectrum *filters- dedicated to a single band of wavelength *monochromators- designed for special scaning (ex: prisms, gratings)

wavelength selector

holds the sample to be analyzed *quartz cuvette- UV or visible region *silicate glass or plastic cell- visible region *nacla or k

sampple cell

-converts radiant energy to a usable elecrical signal *phototubes *photoomultipliers *photoiodides (more sensitive)

radiation detector

displays the transduced electrical signal into number *ex: charge transfer devices

sgnal processor and readout

for analysis of gaeous ions

mass spectrometry

for structure elucidation

NME spectrometry

for quantitative and qualitative analysis

UV-Vis spectromety

for determination of functional groups

atopic absorption specttrometry

-measurement of excess energy lost by emission (flourescence) *thiamine *riboflavin

fluometry

measurement of a transmitted light in a suspension *antibiotics *vitamins

turbidemetry

measurement of reflected light in a suspension

nephelometrry

-a procedure by which solutes are separated by differential migration process in asystem consisting of 2 or more phases components: *stationary *moobile *solute

chromatography

-fixed bed of large surface area --may be aporous orfinely divided solid or a liquid that has been coated in a thin layer of an inert suppoertingmateria -particles should be as small and homogenous as possible

stationary phase

- fluid that moves through or over the surface of the stationary phase -maybe liquid or gas

moble phse

-coponents must be in solution or vapor state -the relative affinity of the solutes for each of the phases must be reversible

solute mixture

-stationary phase -normal phase- sp is polar; mp non polar -reverse phase- sp is non polar; mp is polar

based on natre of sp

*adsorption *partition *on exchange *pore penetration/ permeation *affinity

based on equilibrim process

-the sp is a solid on which th sample is absorbed while the mp may be a liquid or a gas *thin layer chromatography *column chromatography *HPLC *gas chromatography

adsorption chromatography

*SP:solid adsorbent spread thinly on a glass or plstice plate -ex: silica gel, alumina caco3 *MP: organic solvent which is less polar that the SP -ex: hexane, ethyl acetate

thin layer chromatography

based on the determination of retention factors

TLC analysis

used to separate compund from mixture -SP: solid adsorbent packed in a vertical glass column *ex: silica gel, aluminacaco3 -MP: organic slvent aded to the top and flows down through the column -ex: hexane, ethyl silicate

colummn chromatography

-widely usd and preffered currect assay of biological and pharmaceutical product -SP: clumn packed with glass or plastic beads coated with silicone derivatized with non polar functional group

HPLC

if RF is high= non polar if RF is low= polar

normal phase chromatography

-used to analyze volatile substances *SP: either a solid adsorbent or liquid ion in inert support *MP: chemically inert carrier gas (helium or nitrogen)

gas chromatography

-based on partition between 2 immiscible solvents -both SP and Mp are in liquid form

partition chromatography

-SP: water molecules bound to the cellulose of the filter paper -MP: non polar or hydrophobic solvents

paper chromatography

-used for the separation of charged molecule their bindings to fixed charges on a support uses: *most effective method for water purification *separation of amino acid *SP: employs either cationic or anionic exchanger which is capable of exchanging counter ions in the surrounding medim in reversible process

ion exchange chromatography

-molecules are separated according to their site by their ability to penetrate a seive-like structure -ex: size exlusion chromatography

permeation chromatography

utilized, highly specific interactions between one kind of solute moleculeand a second molecule covalently attached to the SP ex: protein affinity chromatography

afffinity chromatography

acetalization method (peppermint- total menthol content))

alcohol

100

bisulfite method (cassia flask) or hydroxyllamine method (titration)

aldehyde and ketone

gastro

Hannah Angelique Losaria · 100問 · 2年前

gastro