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

-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.

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

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

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

-selected or trace compounds

each constituent

--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

what is used in in chemical methods for natural products

what is used in instrumental method for natural products?

what special methods are used for natural products?

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

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

-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

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

-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

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

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

-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

-AKA analyte/active constituents *sample being analyzed

reagents of known concentration -AKA volumetric/standard solution

compounds capabl of changing colors near the end

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)

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

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

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

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

1 titrant

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

-for correction -to enhance the reliability of the endpoint

*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

measurement of an acid by a standard base

*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

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

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

*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

*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

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

volhard titration

volhard VS

primary std used in volhard

indicator in volhard

endpoint in volhard

mohr titration

primary std used in mohr

vs used in mohr

indicator used in mohr

endpoint in mohr

fajans titration

vs used in fajans

primary std used in fajans

en dpoint in fajans

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

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

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

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

point with the maximum upward displacement

point with the maximum downward displacement

the aximum height of a wave

the disance between two identical adjacent point in a wave

the numer of cycles per unit distance

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

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

-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

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

transmittance decrase exponentially as the concentration of the solution increases arithmethically

transmittance decreases exponentially as the thickess of the solution increases arithmethically

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

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

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

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

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

for analysis of gaeous ions

for structure elucidation

for quantitative and qualitative analysis

for determination of functional groups

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

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

measurement of reflected light in a suspension

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

-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

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

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

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

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

-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

*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

based on the determination of retention factors

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

-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

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

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

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

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

-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

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

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

acetalization method (peppermint- total menthol content))

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