Introduction to Modern Liquid Chromatography, Third Edition part 59. High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample. Snyder and Kirkland's Introduction to Modern Liquid Chromatography has long represented the premier reference to HPLC. This Third Edition, with John Dolan as added coauthor, addresses important improvements in columns and equipment, as well as major advances in our understanding of HPLC separation, our ability to solve problems that were troublesome in the past, and the application of HPLC for new kinds of samples. . | 536 METHOD VALIDATION Table Determination of Method Accuracy Recovery and Precision Sample Concentration mg A 11 Accuracy Recovery Replicate 1 Replicate 2 Replicate 3 9 .54 o 981 1 Mean o Standard deviation Relative standaM deviation Acceptance triieria Accuracy mean Precision RSD5 e 98-102 e Assessment Pass Pass product spiked with known amounts of impurities if impurities arenot available see specificity Section . Table illustrates a representative accuracy study. To document accuracy the guidelines recommend that data be collected from a minimum of nine determinations over a minimum of three concentration levels covering the specified range . threeconcenteations threereplicateseoch . TCedatashoulCbe ria accdes the percentrecoverp of thekoown tradded amount or as the difference between the mean and ttae vrlur wibhconfiaenae intervela 1SD . .liable 12T Caic are shownralabiveto hOae e acinitDeaa ae-aveey loai C with RStD o. Ic tiimemooplr aaththaacauoacy aad peeaision pass iee pre-defined a ccptaacea iao i iite0i C iiitl eespetPaely. Prac siD0 The precision 0 enanalytiealmethod ir hefineCas teeclotraesioCagreemeniameng individual teseresuks feom .0 03 analyses oneOomoeentoos is commonly performed as three different measurements repeatability intermediate precision andr odncM t . l . Repeatability it a The abilitt. ofmetetlmethod Caganerate tlo same resulIeoverashoIatSmeintervel under idemticai conDilona intta-aisay precision should be determined from a minimum of nine determinations. Their repeatability should cover the specified range of the procedure . three concentrations three repetitions each or from a minimum of six determinations at 100 of the test or target concentration. RepresentttireeepertcOlliiy multa aee summoriaea mTaCla tl wiieac sesiiits ctC summarizboiat sixeepSicatemjecsions oc Diasame .
