You are hereA REVIEW ON ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF PHARMACEUTICAL TECHNOLOGY

A REVIEW ON ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF PHARMACEUTICAL TECHNOLOGY


7. Limit of quantification:
The limit of quantization is the minimum injected amount that produces quantitative Measurements in the target matrix with acceptable precision in chromatography, typically requiring peak heights 10 to 20 times higher than the baseline noise. If the required precision of the method at the limit of quantization has been specified, the EURACHEM (22) approach Can be used. It is important to use not only pure standards for this test but also spiked matrices that closely represent the unknown samples. For the limit of detection, the ICH (5) recommends, in addition to the procedures as described above, the visual inspection and the standard deviation of the response and the slope of the calibration curve. Figure 3 illustrates the limit of quantization (along with the limit of detection, range and linearity). Figure 4 illustrates both the limit of detection and the limit of quantization.

Figure No 2 Shows Limit of Quantification&Detection

8. Repeatability
From the repeatability standard deviation are it is useful to calculate the ‘repeatability limit ‘r’’, which enables the analyst to decide whether the difference between duplicate analyses of a sample, determined under repeatability conditions, is significant.

9. Measurement uncertainty
Measurement uncertainty is a single parameter (usually a standard deviation with a Coverage factor or confidence interval) expressing the range of values possible on the basis of the measurement result. A measurement uncertainty estimate takes account of all Recognized effects operating on the result; the uncertainties associated with each effect are combined according to well-established procedures. An uncertainty estimate for analytical Chemistry is often termed an ‘uncertainty budget’ and should take into account .The overall, long-term precision of the method;[ 55-56]

·         Bias and its uncertainty, including the statistical uncertainty involved in the bias measurements, and the reference material or method uncertainty. It may be necessary to increase the estimate where a significant bias is detected but left uncorrected.

·         Calibration uncertainties. As most equipment calibration uncertainties will be Negligibly small by comparison with overall precision and uncertainty in the bias; this needs only to be verified;

·         Any significant effects operating in addition to the above. For example, temperature or time ranges permitted by the method may not be fully exercised in validation studies, and their effect may need to be added. Such effects can be usefully quantified by robustness studies (see ‘Ruggedness’ below) or related studies which establish the size of a given effect on the result. Where the contribution of individual effects is important, for example in calibration laboratories.

10. Sensitivity
This is effectively the gradient of the response curve, i.e. the change in instrument response, which corresponds; to a change in analyze concentration. Where the response has been established as linear with respect to concentration, i.e. within the linear range of the method, and the intercept of the response curve has been determined, sensitivity is a useful parameter to calculate and use in formulae for quantization. [57]

11. Ruggedness (or robustness)
Ruggedness is normally evaluated during method development, typically by the originating Laboratory, before collaborating with other laboratories and is a measure how well a method stands up to less than perfect implementation. Performance, and may even result in the method not working at all. These stages should be identified, usually as part of method development, and if possible, their influence on method performance evaluated using ‘ruggedness tests’, sometimes also called ‘robustness tests’[56 57]

CONCLUSION
The efficient development and validation of analytical methods are critical elements in the development of pharmaceuticals. Success in these areas can be attributed to several important factors, which, in turn, will contribute to regulatory compliance. Experience is one of these factors both the experience level of the individual scientists and the collective experience level of the development and validation department .Recent development in pharmaceutical and biotechnological field generates a cumulative demand for analytical methods. Rapid and accurate quantification of the substrate and drug product is important in the process development. Improvements in analytical instrumentation leads to development of new techniques like isocratic and gradient RP-HPLC, which evolved as the primary techniques for the analysis of nonvolatile APIs and impurities. These analytical methods are critical elements of pharmaceutical development so it is very important to develop efficient and accurately validated analytical methods to develop safe and effective drugs. [58]

REFERENCES
1. Swarbrick James., and Boylan James., Encyclopedia of pharmaceutical technology, Volume I, Marcel Dekker Inc., New York, (1998), 217 - 224.
2.Beckett,A.H., Stenlake J.B., Practical Pharmaceutical Chemistry, (1997), 4th edition, Part 2,   CBS Publishers and distributors, 275-337.
3. Glenn A.L., Journal of pharmacy and pharmacology, (1960), 12,598-608.
4.Jain H.K., Agrawal R.K., Indian Journal of pharmaceutical sciences, (2002), 64(1),  88-71.
5.Shankar M.B., Mehta F.A., Bhatt K.K., Mehta R.S., and Geetha M., Indian Journal of pharmaceutical sciences, 65(2), 167-170.
6.Skoog DA, West DM, Holler FJ (1996) Fundamentals of analytical chemistry.       (8thEdn), Fort Worth: Saunders College Pub.
7.Song HH, Choi KS, Kim CW, Kwon YE (2009) Pharmacokinetic Profiles of Two Branded Formulations of Piroxicam 20mg in Healthy Korean Volunteers by a Rapid Isocratic HPLC Method. J Bioequiv Availab 1: 074-079.   
8. Nanjwade BK, Ali MS, Nanjwade VK, Manvi FV (2010) Effect of Compression Pressure on Dissolution and Solid State Characterization of Cefuroxime Axetil. J Anal Bioanal Techniques 1:112.
9. Yue PF, Yuan HL, Yang M, Zhu WF (2009) Preparation, Char-acterization and Pharmacokinetics in Vivo of Oxymatrine-Phospholipid Complex. J Bioequiv Availab 1: 099-102.    
10. Maithani M, Singh R (2011) Development and Validation of a Stability-Indicating  HPLC Method for the Simultaneous Determination of Salbutamol Sulphate and Theophylline in Pharmaceutical Dosage Forms. J Anal Bioanal Techniques 1:116.
11. Chitlange SS, Chaturvedi KK, Wankhede SB (2011) Development and Validation of Spectrophotometric and HPLC Method for the Simultaneous Estimation of Salbutamol Sulphate and Prednisolone in Tablet Dosage Form.  J Anal Bioanal Techniques 2:117.
12. Saber AL, Amin AS (2011) Utility of Ion-Pair and Charge Transfer Complexation for Spectrophotometric Determination of Domperidone and Doxycycline in Bulk and Pharmaceutical Formulations. J Anal Bioanal Techniques 1:113.   
 13.Bai L, Ma Z, Yang G, Yang J, Cheng J (2011) A Simple HPLC Method for the Separation of Colistimethate Sodium and Colistin Sulphate. J Chromatograph Separat Techniq 1:105.
14.Babu ARS, Thippeswamy B, Vinod AB (2011) Determination of Tacrolimus in Rat Whole Blood Utilizing Triple Quadrupole LC/MS. J Anal Bioanal Techniques 2:118.
15.Junior EA, Duarte LF, Pereira R, Pozzebon JM, Tosetti D, et al. (2011) Gabapentin Bioequivalence Study: Quantification by Liquid Chromatography Coupled to Mass Spectrometry. J Bioequiv Availab 3: 187-190.
16.Hsieh CL, Wang HE, Ker YB, Peng CC, Chen KC, et al. (2011) GC/MS Determination of N-butyl-N-(3-carboxypropyl) Nitrosamine (BCPN) in Bladder Cancers - The Skewed Molecular Interaction Caused Retention Time Shift. J Anal Bioanal Techniques 1:115.
17.Ekeberg D, Norli HR, Stene C, Devle H, Bergaust L (2010) Identification of Brominated Flame Retardants in Sediment and Soil by Cyclohexane Extraction and Gas Chromatography Mass Spectrometry. J Chromatograph Separat Techniq1:102
18.Ravali R, Phaneendra M, Bhanu Jyothi K, Ramya Santhoshi L, Sushma K (2011) Recent Trends in Analytical Techniques for the Development of Pharmaceutical Drugs. J Bioanal Biomed R1: 002.
19. M.S. Tswett, TR Protok, Otd. Biol., 14 (1903, publ. 1905) 20.
20.Verzele M, Dewaele C (1985) Preparative High Performance Liquid Chromatography, A Practical Guidline. TEC Dent, Belgium.
21.Dhaneshwar SR, Salunkhe JV, Bhusari VK (2010) Validated HPTLC Method for Simultaneous Estimation of Metformin Hydrochloride, Atorvastatin and Glimepiride in Bulk Drug and Formulation. J Anal Bioanal Techniques 1:109.
22.Abdelkawy M, Metwaly F, El Raghy N, Hegazy M, Fayek N (2011) Simultaneous determination of Ambroxol Hydrochloride and Guaifenesin by HPLC, TLCSpectro densitometric and multivariate calibration methods in pure form and in Cough Cold Formulations. J Chromatograph Separat Techniq 2:112.
23. Bari SB, Bakhshi AR, Jain PS, Surana SJ (2011) Development and Validation of Stability-Indicating Tlc Densitometric Determination of Ropinirole Hydrochloride in Bulk and Pharmaceutical Dosage Form. Pharm Anal Acta 2:125.
24.Jain PS, Khatal RN, Jivani HN, Surana SJ (2011) Development and Validation of TLC-densitometry Method for Simultaneous Estimation of Brimonidine tartrate and Timolol maleate in Bulk and Pharmaceutical Dosage Form.  J Chromatograph Separat Techniq 2:113.
25.Skoog DA, Leary JJ (1992) Principles of Instrumental Analysis. Harcourt Brace College Publishers.
26.Subbaiah PR, Kumudhavalli MV, Saravanan C, Kumar M, Chandira RM (2010) Method Development and Validation for estimation of Moxifloxacin HCl in tablet dosage form by RP-HPLC method. Pharm Anal Acta 1:109.
27. Sultana N, Arayne MS, Naveed S (2011) RP-HPLC Method for Simultaneous Determination of Captopril and Diuretics: Application in Pharmaceutical Dosage Forms and Human Serum. J Chromatograph Separat Techniq 2:109.
28. Krstulovic AM, Brown PR (1982) Reversed-Phase High Performance Liquid Chromatography, Wiley, New York.
29.Sawant L, Prabhakar B, Pandita N (2010) Quantitative HPLC Analysis of Ascorbic Acid and Gallic Acid in Phyllanthus Emblica. J Anal Bioanal Techniques 1:111.
30.El-Sayed AAY, Mohamed KM, Hilal MA, Mohamed SA, Aboul-Hagag KE, et al. (2011) Development and Validation of High-Performance Liquid Chromatography-Diode Array Detector Method for the Determination of Tramadol in Human Saliva. J Chromatograph Separat Techniq 2:114.
31.Reddy YR, Kumar KK, Reddy MRP, Mukkanti K (2011) Rapid Simultaneous Determination of Sumatriptan Succinate and Naproxen Sodium in Combined Tablets by Validated Ultra Performance Liquid Chromatographic Method. J Anal Bioanal Techniques 2:121.
32.Naveen Kumar Reddy G, Rajendra Prasad VVS, Maiti NJ, Nayak D, Prashant Kumar M (2011) Development and Validation of a Stability Indicating UPLC Method for Determination of Moxifloxacin Hydrochloride in Pharmaceutical Formulations. Pharm Anal Acta 2:142.
33.Nanjwade BK, Patel DJ, Parikh KA, Nanjwade VK, Manvi FV (2011) Development and Characterization of Solid-Lipid Microparticles of Highly Insoluble Drug Sirolimus. J Bioequiv Availab 3: 011-015.
34. Yi SJ, Shin HS, Yoon SH, Yu KS, Jang IJ, et al. (2011) Quantification of Ticlopidine in Human Plasma Using Protein Precipitation and Liquid Chromatography Coupled with Tandem Mass Spectrometry. J Bioanal Biomed 3: 059-063.
35. Rajender G, Narayana NGB (2010) Liquid Chromatography-Tandem Mass Spectrometry Method for Determination of Paclitaxel in Human Plasma. Pharm Anal Acta 1:101.
36.Yang G, Liu Y, Liu H, Yang C, Bai L, et al. (2010) Preparation of a Novel Emulsion-Templated MIP Monolith and its Application for on Line Assay of Nifedipine in Human Plasma. J Chromatograph Separat Techniq 1:103.
37.Moreno RA, Sverdloff CE, Oliveira RA, Oliveira SE, Borges DC, et al. (2009) Comparative bioavailability and pharmacodynamic aspects of cyclobenzaprine and caffeine in healthy subjects and the effect on drowsiness intensity. J Bioequiv Availab 1: 086-092.
38. Puri A, Mehdi B, Panda NB, Dhawan GDPS (2011) Estimation of Pharmacokinetics of Propofol in Indian Pateints by HPLC Method. J Anal Bioanal Techniques 2:120.
39.Remsberg CM, Yáñez JA, Vega-Villa KR, Davies NM, Andrews PK, et al. (2010) HPLC-UV Analysis of Phloretin in Biological Fluids and Application to Pre- Clinical Pharmacokinetic Studies. J Chromatograph Separat Techniq 1:101.
40.Sarker SD, Lafont R, Girault JP, Sik V, Dinan L (1998) Pharmaceutical Biology. 36: 202-206.
41. Sievert P, Hancock WS (1996) new methods in peptide mapping for the characterization of proteins, CRC press, Inc., New York.
42.Furusawa N (2001) Determining the procedure for routine residue monitoring of sulfamethazine in edible animal tissues. Biomed Chromatogr 15: 235-239.
43.Guiochon G, Katti A (1987) Preparative Liquid Chromatography. Chromatographia 24: 165.
44. Bao Y, Li C, Shen H, Nan F (2004) Determination of saikosaponin derivatives in Radix bupleuri and in pharmaceuticals of the Chinese multiherb remedy xiaochaihu-tang using liquid chromatographic tandem mass spectrometry. Anal Chem 76: 4208-4216.
45.Liu L, Cheng Y, Zhang H (2004) Phytochemical analysis of anti-atherogenic constituents of Xue-Fu-Zhu-Yu-Tang using HPLC-DAD-ESI-MS. Chem Pharm Bull 52: 1295-1301.
46.Liu SJ, Liu ZX, Jug WZ, Zhou L, Chen M, et al. (2010) Development and Validation of a Liquid Chromatographic/ Mass Spectrometric Method for the Determination of Saikosaponin a in Rat Plasma and its Application to Pharmacokinetic Study. J Anal Bioanal Techniques 1:104.
47. Breda C.A., Breda M., Frigerio E., Bioanalytical method validation: a risk-based approach?, Journal of Pharmaceutical and Biomedical Analysis,35, 2004, 887–89
48.Nakashima Kenichiro, High-Performance Liquid Chromatography of drug of abuse in     biological  samples, Journal of Health Science, 51(3) 272-277 (2005)
49.Boulanger B., Chiap P. Dewe W., Crommen J., Hubert Ph., An analysis of the SFSTP guide on validation of chromatographic bioanalytical methods: progresses and limitations Journal of Pharmaceutical and Biomedical Analysis,32, 2003,753-765
50. Causon Roger, Validation of chromatographic methods in biomedical analysis viewpoint and discussion, Journal of Chromatography B, 689 (1997) 175-180
 51.Hartmann C., Smeyers-Verbeke J., Massart D. L., McDowall R.D., Validation of bioanalytical chromatographic methods, Journal of Pharmaceutical and Biomedical  Analysis17, 1998,193–218
52. G. C. Hokanson, A life cycle approach to the validation of analytical methods during   pharmaceutical product development, Part II: Changes and the need for additional Validation,   Pharm.Tech. Oct. 1994, pp. 92–100.
53. J. M. Green, A practical guide to analytical method validation, Anal. Chem. News &  Features, 1 May 1996, pp. 305A–309A.
54. B. Renger, H. Jehle, M. Fischer and W. Funk, Validation of analytical procedures in  pharmaceutical analytical chemistry: HPTLC assay of theophylline in an effervescent tablet, J. Planar Chrom. 8:269–278 (July/August 1995).
 55. Wegscheider, Validation of analytical methods, in: Accreditation and quality assurance In  analytical chemistry, edited by H. Guenzler, Springer Verlag, Berlin (1996).
56. S. Seno, S. Ohtake and H. Kohno, Analytical validation in practice at a quality control   laboratory in the Japanese pharmaceutical industry, Accred. Qual. Assures. 2:140–145 (1997).
57. AOAC Peer-Verified Methods Program, Manual on policies and procedures, Arlington,
58. A report by Jay Breaux , Kevin Jones  and Pierre Boulas AAI Development    ServicesAnalytical Method Development and Validation

NOW YOU CAN ALSO PUBLISH YOUR ARTICLE ONLINE.

SUBMIT YOUR ARTICLE/PROJECT AT articles@pharmatutor.org

Subscribe to Pharmatutor Alerts by Email

FIND OUT MORE ARTICLES AT OUR DATABASE


FIND MORE ARTICLES

Subscribe to RSS headline updates from:
Powered by FeedBurner