Scribd Logo
Upload

Welcome to Scribd!

  • 30 views

    Method Development Part 2 - Sharing Knowledge HPLC

    Uploaded by

    alfan arbianto
    Terimakasih sudah mendownload. File Audionya dapat di dengarkan di https://linktr.ee/alfan.arbianto.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd

    Method Development Part 2 - Sharing Knowledge HPLC

    Uploaded by

    alfan arbianto
    30 views30 pages
    Terimakasih sudah mendownload. File Audionya dapat di dengarkan di https://linktr.ee/alfan.arbianto.

    Copyright

    © © All Rights Reserved

    Available Formats

    PDF, TXT or read online from Scribd

    Did you find this document useful?

    Is this content inappropriate?

    Terimakasih sudah mendownload. File Audionya dapat di dengarkan di https://linktr.ee/alfan.arbianto.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    30 views30 pages

    Method Development Part 2 - Sharing Knowledge HPLC

    Uploaded by

    alfan arbianto
    Terimakasih sudah mendownload. File Audionya dapat di dengarkan di https://linktr.ee/alfan.arbianto.

    Copyright:

    © All Rights Reserved
    Download as PDF, TXT or read online from Scribd
    Download as pdf or txt
    You are on page 1of 30

    Method Development

    (High Performance Liquid Chromatography)


    by Alfan Danny Arbianto
    OUR GOAL
    • Memahami langkah-Langkah Ketika akan
    melakukan sebuah analisis sampel

    Your Date Your Footer Here 2


    Outline

    Validation
    1 Guidelines
    q Kenali Sampel
    q ICH Guideline

    q Journal

    3 4
    q Pharmacopeia

    Examples

    2 Verification

    Your Date Your Footer Here 3


    Guide Line

    Start from
    q Kenali Sampel
    q Pharmacopeia
    q Journal

    01

    Your Date Your Footer Here 4


    Kenali Sampel

    SAMPEL
    q Jenis &
    karakteristiknya
    q Known Sampel
    Tak Kenal
    q Unknown Sampel maka Tak Sayang
    q Polarity
    q Solubility

    Your Date Your Footer Here 5


    Pharmacopeia
    • Validitas tinggi
    • Hanya perlu verifikasi
    • Waktu developmentnya lebih singkat
    • Mengurangi cost analisa

    Your Date Your Footer Here 6


    Pharmecopeia
    1 Indonesia 3 JP
    Pharmacopeia
    q Physic Analysis
    q Physic Analysis q Chemical Analysis
    q Chemical Analysis

    2 USP 4 EP
    q Physic Analysis q Physic Analysis
    q Chemical Analysis q Chemical Analysis

    http://www.uspbpep.com/

    Your Date Your Footer Here 7


    European Pharmacopeia 6.0

    Your Date Your Footer Here 8


    Informasi
    Penting
    q Solubility
    q Konsentrasi sampel &
    standard
    q Column
    q Detector
    q Flow
    q Run Time

    01
    Column?

    Your Date Your Footer Here 9


    Column HPLC

    https://www.ich.org/page/quality-guidelines

    Your Date Your Footer Here 10


    Journal

    Your Date Your Footer Here 11


    Kondisi HPLC

    Your Date Your Footer Here 12


    Kualitas Peak

    Resolusi Peak

    Peak tailing

    Your Date Your Footer Here 13


    Preparasi Sampel

    Your Date Your Footer Here 14


    Data Validasi

    Your Date Your Footer Here 15


    Data Validasi

    Your Date Your Footer Here 16


    Verification & Validation

    Your Date Your Footer Here 17


    Verification Process
    USP EDQM AOAC
    Specificity Specificity Specificity
    Precision Precision Precision
    Linearity Linearity -
    Range - -
    - Accuracy Accuracy

    Catatan: Karena kompendial bersifat territorial, maka harus dilihat secara


    detail dan akan berbeda beda persyaratan serta batas nilai yang di ijinkan

    Your Date Your Footer Here 18


    Validation Process
    Based on ICH guideline Protocols

    Your Date Your Footer Here 19


    Validation Process
    Based on ICH guideline Protocols

    Your Date Your Footer Here 20


    Specificity
    Specificity is the ability to assess unequivocally the analyte in the
    presence of components which may be expected to be present.
    Typically these might include impurities, degradants, matrix, etc.

    Your Date Your Footer Here 21


    Linearity
    The linearity of an analytical procedure is its ability (within a given
    range) to obtain test results which are directly proportional to the
    concentration (amount) of analyte in the sample.

    Your Date Your Footer Here 22


    Range
    The range of an analytical procedure is the interval between the
    upper and lower concentration (amounts) of analyte in the
    sample (including these concentrations) for which it has been
    demonstrated that the analytical procedure has a suitable level of
    precision, accuracy and linearity.

    Your Date Your Footer Here 23


    Accuracy
    The accuracy of an analytical procedure expresses the closeness
    of agreement between the value which is accepted either as a
    conventional true value or an accepted reference value and the
    value found.

    Your Date Your Footer Here 24


    Precision
    The precision of an analytical procedure expresses the closeness of
    agreement (degree of scatter) between a series of measurements
    obtained from multiple sampling of the same homogeneous sample
    under the prescribed conditions. Precision may be considered at three
    levels: repeatability, intermediate precision and reproducibility

    Your Date Your Footer Here 25


    LOD & LOQ
    Detection Limit, The detection limit of an individual analytical
    procedure is the lowest amount of analyte in a sample which can
    be detected but not necessarily quantitated as an exact value

    Quantitation Limit, The quantitation limit of an individual


    analytical procedure is the lowest amount of analyte in a sample
    which can be quantitatively determined with suitable precision
    and accuracy

    Your Date Your Footer Here 26


    Cara? LOD & LOQ
    Standard stock solutions of cefotaxime sodium (6.25, 12.50, 25, 50,
    100, and 200 μg/mL were prepared) by diluting the standard stock
    solution (1000 ppm) with mobile phase.

    Your Date Your Footer Here 27


    Robustness
    The robustness of an analytical procedure is a measure of its
    capacity to remain unaffected by small, but deliberate variations
    in method parameters and provides an indication of its reliability
    during normal usage.

    Your Date Your Footer Here 28


    System Suitability Testing

    Your Date Your Footer Here 29


    Q&A

    Your Date Your Footer Here 30

    You might also like