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Validasi dan Verifikasi Metode Analisis

Validasi dan Verifikasi Metode Analisis. Alfas – Surabaya, 29 Maret 2014. Mochammad Yuwono Fakultas Farmasi Universitas Airlangga E-mail: yuwono05@yahoo.com. Sharing Knowledge Ikatan Alumni Universitas Airlangga – Fakultas Farmasi. Quality. Efficacy. Safety.

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Validasi dan Verifikasi Metode Analisis

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  1. ValidasidanVerifikasiMetodeAnalisis Alfas – Surabaya, 29 Maret 2014 MochammadYuwono FakultasFarmasiUniversitasAirlangga E-mail: yuwono05@yahoo.com Sharing Knowledge Ikatan Alumni UniversitasAirlangga – FakultasFarmasi

  2. Quality Efficacy Safety Quality is important in every product or service, but it is vital in medicines as it involves life. RegulasiObat: PersyaratanSangatketat ! Sharing Knowledge

  3. Quality Invisible when GOOD Impossible to ignore when BAD • How good something is • If the quality of a product is low, it means that the product is not really good Sharing Knowledge

  4. Quality of Products • The ability to make the same product the same way, over and over again. • Customer buys today is same as what they bought last month or will buy next month. Consistent • Product meets customer’s expectation. reliable Sharing Knowledge

  5. Quality of Pharmaceutical Products Motivation Machine Man Methods calibrated qualified characterised documented robust suitable skilled qualified Quality of thepharmaceutical products Referencestandards Vibrations Time Analysts´support Irradi-ations Tempe-rature Supplies Humidity Quality Material Milieu Management Measurements Sharing Knowledge

  6. Quality in Analytical Laboratory Akomodasi & Lingkungan Analis Baku Pembanding, Reagensia Pendidikan Pelatihan Pengalaman Hasil Valid & Terpercaya Preparasisampel VerifikasiKinerja Presisi Kualifikasi Validitas Linieritas Akurasi, LOD, LOQ Linieritas Alat/Instrumen Sensitvitas Selektivitas Kalibrasi SST MetodeAnalisis Sharing Knowledge

  7. Quality of Analytical Data HirarkiKomponenMutu Data Analisis Internal QA (Sampelkontrolmasukrentang) Sistem (memenuhiuji SST) MetodeAnalisis (telahdivalidasi/diverifikasi) InstrumenAnalisis (memenuhikualifikasi DQ, IQ, OQ, PQ) Sharing Knowledge

  8. VALID & TERPERCAYA Safety Pengelola & Analis Sampel Dokumensistem Mutu MetodeAnalisis Alat/ Instrumen Sarana & Prasarana Bahan Kimia & SRM SistemManajemenMutu Sharing Knowledge Laboratorium QC

  9. Analisis ProsedurAnalisis PengembanganMetode Validasi /VerifikasiMetode Quality Assurance: ISO 17025/GLP SampelObat, ObatTradisional, Makanan, Kosmetik LaporanHasil PreparasiSampel– Analisis data Sampling Sharing Knowledge

  10. MetodeAnalisisKlasik • Spot test • Volumetri/Titrasi (menggunakanindikator) Metode Instrumental Spektrometri(UV-Vis, IR, AAS, ICP) Elektrokimia (Potentiometri, ISE dll) MS, NMR MetodePemisahanKromatografi (HPLC, GC,TLC, CE dll) MetodeAnalisis Kimia Hyphenated Instruments GC-MS GC-FTIR/MS LC-MS/MS LC-NMR Sharing Knowledge

  11. MetodeAnalisis Pengembangan Optimasi Pre-validasi Validasi Revalidasi Andev Implementasi (rutin) QC Sharing Knowledge

  12. MetodeStandar/Baku Single Laboratory Validation Full Validation • In House Validation of Method • Interlaboratory Validation • (Collaborative Study) • Standard Method • Verification of Method Sharing Knowledge

  13. Compendial Methods • Metode yang terteradalamFarmakope • MerupakanmetodeStandar yang telahdivalidasi (Full Validation) • TermasukmetodeResmi (Official method) untuknegara-negaratertentu Sharing Knowledge

  14. KategoriMetodeAnalisis Penetapankadarkomponenutama dalambahanbakuobatataubahan aktifdalamsediaanfarmasi I Penetapancemaranatauhasil Degradasi Penetapankuantitatif (II a) danujibatas/kualitatif (II b) Kategori MetodeAnalisis (USP) II III Penetapankarakteristiksediaan (disolusi, pelepasanobat, dll) IV Metodeanalisisuntukidentifikasi Sharing Knowledge

  15. KarakteristikkinerjametodeUSP dan ICH Presisi Akurasi Batas Deteksi (DL/LOD) ValidasiMetode Batas Kuantitasi (QL/LOQ) Selektivitas/Spesifisitas Linieritas Rentang Robustness/Ruggedness System Suitability Test Sharing Knowledge

  16. Parameter ValidasiMenurut USP dan ICH Sharing Knowledge

  17. Akurasi dan Presisi Metode AkurasirendahPresisitinggi Akurasi tinggi Presisi tinggi AkurasitinggiPresisirendah (Hasildirata-rata) Akurasi rendah Presisi rendah Sharing Knowledge

  18. TahapanValidasiMetode Literature search TelaahkarakteristikAnalit Penyiapanbahandanalat Pengembangan/ optimasiMetode PembuatanprotokolValidasi PermintaanValidasi Validasi Metode Penyerahandokumen Percobaanlaboratoriumsesuaiprotokolvalidasi PenyusunanLaporanValidasi Analisis Data Sharing Knowledge

  19. ValidasiMetode Vs. VerifikasiMetode Sharing Knowledge

  20. Verifikasi • Suatuproses(percobaan • laboratorium) • Untukmembuktikanbahwa • karakteristikkinerjametode • analisistelahmemenuhi • persyaratan yang telahditetapkan • sebelumnya Validasi • Suatuproses(percobaan • laboratorium) • Untukmembuktikanbahwa • laboratoriummampu • menggunakanmetodeanalisis • baku/standarpadakondisinyata di • laboratoriumnya Sharing Knowledge

  21. Metodebaku/Standar Compendial Method (USP, FI, AOAC, ISO dll.) Verifikasi • Metodetidakbaku • Metodepengembangan • Metodebaku yang • dimodifikasi • Metodebaku yang • digunakandiluar • lingkup Validasi Sharing Knowledge

  22. Modifikasimetodekompendial • Jikapadaverifikasimetode, kondisipadaMetodekompendial TIDAK diperolehhasil yang optimal (misal peak tailing, fronting, splitting, resolusipemisahantidakterpenuhi)  Laboratoriumdapatmelakukanmodifikasiatau adjustment. • Pada USP terterabatas-batasmodifikasiatau adjustment yang diperkenankan Sharing Knowledge

  23. Modifikasi/Adjustment metodekompendial Sharing Knowledge

  24. Panduanvalidasimetodeanalisis • ICH Q2A : Text on validation of analytical Procedure • ICH Q2B Validation of analytical procedures methodology • FDA-CDER (Center for Drug Evaluation and Research) • Reviewer guidance validation of chromatographic methods • b. Submitting sample and analytical data for method validation • Analytical procedure and method validation for human studies • Bioanalytical method validation for human studies • USP: Validation of compendial procedures • USP: Verification of compendial procedures Sharing Knowledge

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  28. VerifikasiMetode • Adopsimetodebaku/standar • Untukmembuktikanbahwasuatulaboratorium mampumelakukananalisisdilaboratoriumnya • untukmenunjukkanbahwakinerjametodedapatditiruataudiulangolehlaboratorium yang bersangkutandenganhasil yang sama Sharing Knowledge

  29. Metodebaku/Standar Compendial Method (USP, FI, AOAC, ISO dll.) Verifikasi • Metodetidakbaku • Metodepengembangan • Metodebaku yang • dimodifikasi • Metodebaku yang • digunakandiluar • lingkup Validasi Sharing Knowledge

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  32. Metode “General Test” (LOD, sisapijar, bilanganasam, pH) tidakperludiverifikasi Sharing Knowledge

  33. AcuanVerifikasiMetode Sharing Knowledge

  34. KategoriAnalisis Confirmation of Identity, a method that ensures a material is what it purports to be or confirms the detection of the target analyte. 2. Quantifying an analyte at a low concentration. Determining if an analyte is present above or below a specified, low concentration (often called a Limit Test). The specified concentration is close to the LOQ. 4. Quantifying an analyte at a high concentration. 5. Determining if an analyte is present above or below a specified, high concentration (often called a Limit Test). The specified concentration is substantially above the LOQ. 6. Qualitative test. Sharing Knowledge

  35. Parameter Validasi Sharing Knowledge

  36. Parameter Verifikasi Sharing Knowledge

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  41. Parameter VerifikasiMetode Penetapankadarbahanaktifdalamsediaanfarmasi Selektivitas/spesifisitas, Presisidanakurasimerupakan parameter penting Sharing Knowledge

  42. Selektivitas vs. Spesifisitas USP dan ICH  menggunakanistilah Specificity IUPAC dan AOAC  menggunakanistilah Selectivity AOAC: Specificity  “highest selectivity” Sharing Knowledge

  43. Specificity (ICH/USP) Specificity (USP/ICH): The ability to assess unequivocally the analyte in the presence of components to expected to be present, such as impurities, degradation products, and matrix components. Selectivity describes the ability of an analytical method to differentiate various substances in a sample. Sharing Knowledge

  44. Spesifik dan Selektif Selektif: Mampumembedakanantarasenyawaanalitdenganderivat/degradan/ metabolitatausenyawapengganggulainnya Spesifik: Mampumengenalresponsuntukanalittunggal/murni Sharing Knowledge

  45. Spesifisitas/Selektivitas: Jikatersediazathasildegradasi: Suntikkan: • Blankosampel/Placebo (Sampel minus analit) • ZatHasildegradasi (degradants) • Zat yang memilikistrukturmirip (Related substances • Zat metabolit (untuk bioanalisis) Sharing Knowledge

  46. Spesifisitas/Selektivitas: • Blankosampel/Placebo tidakmenghasilkan peak/nodadenganwakturetensi/Rf yang samadengananalit • Peak/nodaanalitterpisahdari peak/nodalainnya (Rs ≥1,5) Sharing Knowledge

  47. Placebo Sampel (Rs ≥1,5) Sharing Knowledge

  48. Meloxicamdalam tablet (spektrofotometri UV/Vis) Sharing Knowledge

  49. Specificity/Selectivity: • Lakukan forced degradation studies (studidegradasipaksa) • Sampeldisimpanpadasuhu/kelembabantertentuataupenambahanoksidator • Bandingkanprofilpemisahan peak sebelumdansesudahperlakuan Jikatidaktersediazathasildegradasi (Degradants) Sharing Knowledge

  50. Forced Degradation Studies • Heat Temperature (50 - 60 oC) • Humidity Kelembaban (70 to 80%) • Acid Hydrolysis HCl 0.1 N • Base Hydrolysis NaOH 0.1 N • Oxidation H2O2 (3 to 30%) • Light UV/Vis Sharing Knowledge

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