The importance of IR spectroscopy cover a wide range of subjects in pharmacy 1. PHARMACEUTICS :- To check the incompatability studies in between the drug and in-active ingredients in the dosage forms. 2. PHARMACEUTICAL CHEMISTRY :- For the charecterization of the newly synthesized compounds. 3. PHARMACEUTICAL ANALYSIS :- For the qualitative and quantitative study parameters. 4. PHARMACOGNOSY :- For the estimation of natural products by Near-IR spectroscopy and for the structural elucidation of compounds. 5. PHARMACOLGY :- The confirmation of functional groups or basic nucleus of the sample will give basic idea for the acivity ex. if sulphonamide present it is having some antibacterial activity. thank you, the above summerised information got from the following References:- 1. Douglas A.Skoog, F.James Holler, Timothy A.Nieman, ,"Infrared spectroscopy", introduction to instrumental methods of analysis", principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 406. Print. 2. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print. 3. B.K. SHARMA," Infrared spectroscopy" Spectroscopy 20th edition, page no.S-220, goel publications, Delhi, 2007.print.

1.in enantiomers there is no changes or substitution in functional groups but the positions alter will not make any drastic changes in dipolemoment( basic need for exhibiting IR spectrum) hence optical isomers or enatiomers have identical absorption curves. 2.The use of Slow scan interferometer and Rapid scan interferometer will make high resolution IR spectroscopy i.e FT-IR and it is an advansed technique for IR. applications of FT-IR over IR Spectroscopy a. FT-IR gives better spectrum at a resuolution of 4 cm-1. b. examine small size samples c. digital computer data, allows the spectrum of pure compuond to be substracted easily from that of a mixture, easy for component assesment. d.FT-IR measure whole spectrum with accuracy at a time but IR measure only resolution time. thank you for your response , all the above summerized data got from 1.B.K. SHARMA,"infra red spectroscopy " ,spectroscopy ,20th edition, page noS-194, Goel publications, Delhi, 2007. print. 2.Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print.

in preformulation studies IR spectral studies gives an idea of 1. solvent effects i.e solvent--solute interaction studies. 2. id. of organic compounds . 3. detection of impurities 4. kinetic study i.e reactions progress 5. distinction b/t intra and itermolecular H- baonds. 6. study of chemical reactions i.e photlysis 7. study of isomerism in formulation studies IR spectral studies gives an idea of 1. to minimize the incompatability of drugs with inactive ingredients. 2. to control the recations of drugs and other ingredients like millard's action i.e in b/t amines and metalic stearates in presence of lactose . that effects dissolution parameters. 3. for the optimization of formulation development. in post formulation aspects IR spectral studies gives an idea of 1. qualitative 2. quantitative parts i.e quality control see the conclusion slide all the summerized information got from 1. B.K. SHARMA," Infrared spectroscopy" ,spectroscopy ,20th edition, Goel publications, Delhi, 2007. print. 2. Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print. 3.Y.R.Sharma,"infrared spectroscopy", Elementary organic spectroscopy principles and chemical applications, first edition 1980, reprint 2007. print.

IR is both qualitative and quantitative Qualitative analysis ORGANIC COMPOUNDS A. Identification of molecules or functional groups. B. Determination of molecular structure. C. Studying rate of reaction. D. Detection of impurities. E. Isomerism . F. Hydrogen bonding. IN-ORGANIC COMPOUNDS A. High modes of vibrations. B. Lower symmetry of complexes C. Formation of chelates. D. Presence of water. quantitaive analysis 1. calibration curve method 2. baseline method 3. difference method 4. simultaneous method as like UV. 1. B.K. SHARMA," Infrared spectroscopy" Spectroscopy 20th edition, page no.S-220, goel publications, Delhi, 2007.print. 2. Douglas A.Skoog, F.James Holler, Timothy A.Nieman, ,"Infrared spectroscopy", principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 406. Print. 3. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print.

solvents are carbon disulfide carbon tetrachloride chloroform deuterium hydroxide nujol for solid samples etc.. see also instumentation slide

reflecting type gratings or filter grating or prism grating type or Littrowmount prism can be used for dispersive systems in FTIR ( non- dispersive systems ) Michelson interferometer is used Prism monochromator near IR -LiF2 / CaF2----1-5u middle IR - Nacl--2.5--15u far IR - KBr / CsBr---15--40u surface of prism should be smooth to prevent scattering of light. Grating monochromator Reflection gratings:- more preferred ---greater resolution Transmitted gratings :- not used much Adv. of grating over monochromators:- 1.Linear dispersion 2.Used over considerable wavelength ranges. 3. They resist attack of water. 1. Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print. 2. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print.

the commonly used detectors or transducers in IR spectrophotometry are in the order thermal detectors. 1. thermocouple 2. thermistor 3. pyroelectric 4. golay photon detectors 1. photo conductive 2. photovoltaic Thermal detectors:- 1.Thermocouple and Thermopile ---- Voltage induced at the junction of two dissimilar materials. 2. Thermister --- Electric resistance. 3. Pyro electric ---Electric polarization. 4. Golay Cells --- Expansion of solid, gas/liquid. 5.Bolometer ---- Electric resistance. Photon Detectors:- 1.Photo conductive detector --- Conductance 2.Photo Voltaic detector--- Voltage. Miscellaneous Detectors:- 1. Lead tin telluride detector 2. Mercury Cadmium Telluride (MCT) detector 3. Fourier transform see slide no 19 for more information. thank you, for your response. all the above summerized information got from:- 1.Douglas A.Skoog, F.James Holler, Timothy A.Nieman, " Infrared spectroscopy", introduction to instrumental methods of analysis, principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 408-410. 2006 Print. 2. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print

thank you, Near infrared spectroscopy:- sailent features of Near IR:- > Near IR is also called as ' electron band spectra' as this region is very close to UV region. > The range of Near IR in EMR spectrum is 0.75-2.50 um 750--2500 nm 13,300-4000 cm- absorbance of this region observes overtones and combinations of fundamental bands that observed in middle IR. > measures the diffusive reflectance absorption. > Near IR associates with functional groups contain 'H' atom i.e C-H, N-H, O-H, P-H, S-H Streching and bending vibrations. > bands of C=O,C-C,C-F,C-Cl. are abscent. > used for quantitative rather than qualitative. > the common solvents used must not contain any 'H'atom in it.ex. CCL4, CS2,CO2, etc.. > the carbohydrates and protiens can be detected by Near IR. > theory supporting -- Frank codon principle > observed changes -- Excitation, vibration > instrument detector ----------- source of light ------ optical system ----- type of samples Photo conductance----- Tungsten filament ------ Prism grating ----- Solid / liquid ------------------------Nernest glower------------------------------------------------- > optimum for single bonded groups. > mixture of aromatic amines can be easily detected. > water analysis in glyserin, freon, organic films, acetone and fuming nitric acid done by this method. for the more information please see the slide no(s). 7, 8, 10. thank you. all the summerized information got from 1. Roger E. schirmer "infrared methods of analysis",Modern methods of pharmaceutical analysis, 2nd edition,volume 1, published by CRS press, in 1991, Boca Raton, Ann Arbor, Boston, 2000. Print., 2.B.K. SHARMA," Infrared spectroscopy" Spectroscopy 20th edition, page no.S-220, goel publications, Delhi, 2007.print. 3. Douglas A.Skoog, F.James Holler, Timothy A.Nieman, ,"Infrared spectroscopy", principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 406. Print. 4. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print.

thank you drug excipient interactions can be studied by IR peaks and are majorly depends on the a. fuctional groups present in drug b. reactable groups of excipients. if nature of excipient not known the following guidline is preferable 1. the IR spectrum of drug only will helps the functional groups present in it.i.e initial step. 2. the spectrum of drug with excipient ofter the prescribed consequtive periods (time limt) from the date of manfacture will be taken . 3. compare the 1st with 2nd and difference in peaks observed. 4. the difference peak was determined based on the literature avilable. examples the drug excipient interactions may leads to ( some of the examples ) a. weak combination and overtone bands in the region of 2000-1600 cm-1. it is because of substitution pattern of rings molecules . b. metal ligand complexes observed at 200-600cm-1 c. convertion of amide groups to lactum a wider functional groups variation. d. molecular interation problems i.e hydrogen bonding. impurity detection by IR peaks very impure samples often give blurred, indistinct spectra. for detection of impurities is same as per the above and some examples given below 1. presence of p-hydroxy benzoic acid in salicylic acid id by two different peaks 1680, 1665cm-1 respectivly. 2. cyclohexanone as impurity in cyclohexanol on account of its intense c=o absorption band thank you all the summerized information( books only) got from the 1.B.K. SHARMA," Infrared spectroscopy" ,spectroscopy ,20th edition, Goel publications, Delhi, 2007. print. 2. Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print. 3.Y.R.Sharma,"infrared spectroscopy", Elementary organic spectroscopy principles and chemical applications, first edition 1980, reprint 2007. print.

WAVE LENGTH---- WAVE NUMBER-------FREQUENCY RANGE l (mm) ---- y (cm-1) ------- Hz MIDDLE---2.5 - 50 ---- 4000 - 200 ------- 1.2x1014 - 6x112 most of the drugs are identified in these region only as the fucntional groups absorb IR radiations here only. ref:- 1.Douglas A.Skoog, F.James Holler, Timothy A.Nieman, ,"Infrared spectroscopy", introduction to instrumental methods of analysis", principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 406. Print.

FTIR spectroscopy with following provisionals a. interferometers b. sources of error associated in the transformation of digital information on the interferogram into a spectrum. c. FTIR computation of digital spectral data to actual spectrumd. d. apodization. Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print.

in the assesment of drug action the main role is played by the functional groups present in the drug structure. in order to predict the type of activity of drugs we need to id the functional groups i.e done by IR spectroscopy. in comparision with other methods (spectroscopic) the difference in the functional groups will vary the dipole moment and taken as the basis for better interpretaion by IR rather than other. UV-- estimation in presence of any chromophores or auxochromophores NMR-- type of protons and the positional arrangement MASS-- molecular wieght hence, most of the part in structural elucidation is done by IR

Erbium-Doped Fiber Amplifier is commonly used Lock-in Amplifier The signal from the Baratron is passed through a home-built differential dc amplifier, which gives a thirty times gain on the signal, and into the lock-in amplifier. The lockin amplifier is a Stanford Research Systems model SR5 10. It receives the alternating voltage output from the Baratron corresponding the IR-on (chopper open) and IR-off (chopper closed). The reference signal is the voltage signal from the counter which corresponds to the chopper frequency. The sample signal is modulated, filtered and then cross-correlated with the reference frequency. The Baratron signal passes through a low band-pass filter, producing an intensified output signal from the lock in amplifier [Ewing 1997] after establishing the best phase shift to use (between chopper signal and detector signal). The lock-in amplifier produces a flat baseline from the differences in the two measured signals from the Baratron. This removes the requirement to mathematically subtract the increasing (or decreasing) baseline. The baseline contains a large amount of random noise which can be removed either by mathematically averaging the data, or by reducing the sensitivity on the lock-in amplifier to give reduced noise. However, this noise does not cause problems during data collection or analysis. http://ir.canterbury.ac.nz/bitstream/10092/2160/1/Thesis_fulltext.pdf

the commonly used detectors or transducers in IR spectrophotometry are in the order thermal detectors. 1. thermocouple 2. thermistor 3. pyroelectric 4. golay photon detectors 1. photo conductive 2. photovoltaic Thermal detectors:- 1.Thermocouple and Thermopile ---- Voltage induced at the junction of two dissimilar materials. 2. Thermister --- Electric resistance. 3. Pyro electric ---Electric polarization. 4. Golay Cells --- Expansion of solid, gas/liquid. 5.Bolometer ---- Electric resistance. Photon Detectors:- 1.Photo conductive detector --- Conductance 2.Photo Voltaic detector--- Voltage. Miscellaneous Detectors:- 1. Lead tin telluride detector 2. Mercury Cadmium Telluride (MCT) detector 3. Fourier transform see slide no 19 for more information. thank you, for your response. all the above summerized information got from:- 1.Douglas A.Skoog, F.James Holler, Timothy A.Nieman, " Infrared spectroscopy", introduction to instrumental methods of analysis, principles of instrumental analysis, 5th edition, saunders Golden sunburst series. Forth worth, Philadelohia, Chicago, Sydney, Toronto. Page no. 408-410. 2006 Print. 2. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print

1. formation of side lobes or podes and their removal (apodiaztion) 2. error due to difference in sample intervels and phase correction 3. use of type of interferometer. 4. signal to noise ratio 5. sensitivity and kind of detectors, source used 6. operating system these parameters will effect id of compounds Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print

we can find the functional group(s) in the new drug structure if present by IR example suppose a new drug x-spectrum shows various peaks at > 3600--3000cm-1 ---OH, --NH2 , >NH, ?C-H. > 3200--3000cm-1 ?C-H, Ar-- C-H. >3000--2500 cm-1 --C--H of methyl/methelene asymmetric stre. --C--H, --COOH >2300--2100 cm-1 Alkynes 2210---2100 Cyanides 2260--2200 Isocyanides 2280--2250 >1900--1650 cm-1 strong bands--- >c=o---1725--1760 anhydrides ----- 1850---1740 Imides ------ two broad band at 1700 also pls see slide no. 38,39,40

the dipole moment of a system not only depends on the functional groups but also the surroundig groups no two compounds have same D.M but same for enantiomers.we can differentiate the functional groups of same in two different drugs

Expanction of gases at junction pls see the slides

reflecting type gratings or filter grating or prism grating type or Littrowmount prism can be used for dispersive systems in FTIR ( non- dispersive systems ) Michelson interferometer is used Prism monochromator near IR -LiF2 / CaF2----1-5u middle IR - Nacl--2.5--15u far IR - KBr / CsBr---15--40u surface of prism should be smooth to prevent scattering of light. Grating monochromator Reflection gratings:- more preferred ---greater resolution Transmitted gratings :- not used much Adv. of grating over monochromators:- 1.Linear dispersion 2.Used over considerable wavelength ranges. 3. They resist attack of water. 1. Jag Mohan ,"infrared spectroscopy", Organic Spectroscopy, Principles And Applications, 2ndedition,Narosa,Newdelhi, Chennai 2005. Print. 2. Hobart H. Willard, Lynne L. Merritt. Jr., John A. Dean, Frank A. Settle, Jr. "Infrared spectroscopy", instrumental methods of analysis,7thedition page288,289,292,293, content no. 11.1 . CBS publications, Toronto. 2005. print.

Solids 50 to 200 mg is desirable, but 10 mg ground with transparent matrix (such as KBr) is the minimum for qualitative determinations; 1 to 10 mg minimum is required if solid is soluble in suitable solvent. Liquids 0.5 mL is needed if neat, less if pure. Gases 50 ppb http://www.prenhall.com/settle/chapters/ch15.pdf

calibration, SOP's of an instrument is varies from company to company but general guidelines of calibration of IR inlcude a. checking of the radiation source b. checking of RH of surronding c. correction of gass related peaks. d. checking of detectors functioning e. performance of Infrared Cells f. performance of Sealed Cells g. calibration of spectrum of sample with standard. general guidelines for Care And Calibration Of Infrared Cells While most cells used in infrared (IR) spectrophotometers are low in cost compared to the basic instrument, they are not inexpensive. A little extra care will enable IR cells to be used for years. Most IR crystals are hygroscopic, and should be stored in a low humidity area, such as a desiccator. Less than 35% relative humidity is desirable. The useful frequency range of IR materials is listed in McCarthy Application Sheet No. 1. IR cells are usually filled with a hypodermic syringe. When filling cells, do it slowly and gently. Fast filling builds up tremendous pressure inside the cell resulting in a cell that leaks. Place the cell into the instrument and run the spectrum immediately in case the cell leaks or a volatile sample evaporates. Clean the cell right after running the spectrum to prevent damage to the crystals. As a general guideline use a 0.025 mm pathlength cell for a 100% solution, a 0.10 mm pathlength for a 10% solution and 1.0 mm pathlength for a 1% solution. Remove the sample solution by pulling as much sample out as possible with a hypodermic syringe and then blow dry air through the cell with an IR Cell Cleaner (Part# 030) or a syringe. A vacuum can also be drawn gently through the cell to remove the sample. If the sample is a mixture, rinse the cell with the solvent used in the mixture and then blow dry air through the cell. When the cell is clean, put it back into a desiccator to prevent fogging. The pathlength of new cells should be calibrated when received and then checked periodically as the pathlength can increase with use. Calibration Of Sealed Cells The thickness of infrared sealed cells can be measured accurately by the interference fringe method. Any infrared spectrophotometer will do. Adjust the spectrophotometer for a 100% T run. Put the empty cell into the cell holder in the sample beam. Scan through a wide enough frequency range to get at least ten fringes. For linear wavelength instruments, Long pathlength cells, 1.0 mm or greater, will not show a fringe pattern on low resolution spectrophotometers. These long pathlength cells can be calibrated by measuring the absorbance of some bands in a liquid sample. The absorbance of these bands can then be compared to the absorbance of the same bands measured in a shorter pathlength cell. The pathlength of a 0.1 mm or 0.2 mm cell can be measured by the interference fringe method. The short pathlength cell is filled with a liquid sample and the absorbance of some weak and medium intensity bands is measured. Then the long pathlength cell is filled with the same liquid and the absorbance of the same bands is measured. By using Beer's Law and taking a ratio of the absorbance, the pathlength can be calculated for more informaton pls reffer www.mccarthyscientific.com web march 26 2010 www.aspbooks.org. web march 26 2010. www.springerlink.com web march 26 2010.

Coupling of two fundamental vibrations produces two new modes of vibrations with frequency higher and lower than that observed in absence of interaction. Interaction between fundamental vibrations and overtones or combinational overtones is called Fermi resonance.

Solids 50 to 200 mg is desirable, but 10 mg ground with transparent matrix (such as KBr) is the minimum for qualitative determinations; 1 to 10 mg minimum is required if solid is soluble in suitable solvent.