Design of Experiments (DoE) is an indispensable tool in contemporary drug analysis as it
simultaneously balances a number of chromatographic parameters to ensure optimal separation
in High Pressure Liquid Chromatography (HPLC). This manuscript briefly outlines the theoretical
background of the DoE and provides step-by-step instruction for its implementation in HPLC
pharmaceutical practice. It particularly discusses the classification of various design types and
their possibilities to rationalize the different stages of HPLC method development workflow, such
as the selection of the most influential factors, factors optimization and assessment of the method
robustness. Additionally, the application of the DoE-based Analytical Quality by Design (AQbD)
concept in the LC method development has been summarized. Recent achievements in the use of
DoE in the development of stability-indicating LC and hyphenated LC-MS methods have also
been briefly reported. Performing of Quantitative ...structure retention relationship (QSRR) study
enhanced with DoE-based data collection was recomended as a future perspective in description
of retention in HPLC system.
Dizajn eksperimenata (DoE) je nezaobilazan alat u savremenoj analizi lekova budući da istovremeno balansira niz hromatografskih parametara kako bi se osiguralo optimalno razdvajanje u tečnoj hromatografiji pod visokim pritiskom (HPLC). Prikazana je teorijska osnova DOE i data su detaljna uputstva za njegovu primenu u HPLC ispitivanjima u farmaciji. Naročito se govori o klasifikaciji brojnih tipova dizajna i njihovim mogućnostima za racionalizaciju različitih faza tokom procesa razvoja HPLC metode, kao što su izbor najuticajnijih faktora, optimizacija faktora i procena robusnosti metode. Dodatno, sumirana je primena DOE kao sastavnog dela koncepta ugradnje kvaliteta u proizvod u domenu razvoja analitičkih metoda (AQbD) zasnovanih na HPLC tehnici. Takođe su prikazana i nedavna dostignuća u primeni DOE u razvoju LC metoda koje su pogodne za ispitivanje stabilnosti lekova, kao i LC-MS metoda. U budućoj perspektivi, preporučeno je izvođenje ispitivanja kvantitativnog odnosa između strukture... i retencionog ponašanja (QSRR) analita u HPLC sistemu na osnovu podataka dobijenih primenom DOE.
Keywords:
Design of experiments / drug analysis / high pressure liquid chromatography / analytical method development and validation / eksperimentalni dizajn / analitika lekova / tečna hromatografija pod visokim pritiskom / razvoj i validacija analitičke metode
TY - JOUR
AU - Stojanović, Jevrem
AU - Krmar, Jovana
AU - Protić, Ana
AU - Svrkota, Bojana
AU - Đajić, Nevena
AU - Otašević, Biljana
PY - 2021
UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/3951
AB - Design of Experiments (DoE) is an indispensable tool in contemporary drug analysis as it
simultaneously balances a number of chromatographic parameters to ensure optimal separation
in High Pressure Liquid Chromatography (HPLC). This manuscript briefly outlines the theoretical
background of the DoE and provides step-by-step instruction for its implementation in HPLC
pharmaceutical practice. It particularly discusses the classification of various design types and
their possibilities to rationalize the different stages of HPLC method development workflow, such
as the selection of the most influential factors, factors optimization and assessment of the method
robustness. Additionally, the application of the DoE-based Analytical Quality by Design (AQbD)
concept in the LC method development has been summarized. Recent achievements in the use of
DoE in the development of stability-indicating LC and hyphenated LC-MS methods have also
been briefly reported. Performing of Quantitative structure retention relationship (QSRR) study
enhanced with DoE-based data collection was recomended as a future perspective in description
of retention in HPLC system.
AB - Dizajn eksperimenata (DoE) je nezaobilazan alat u savremenoj analizi lekova budući da istovremeno balansira niz hromatografskih parametara kako bi se osiguralo optimalno razdvajanje u tečnoj hromatografiji pod visokim pritiskom (HPLC). Prikazana je teorijska osnova DOE i data su detaljna uputstva za njegovu primenu u HPLC ispitivanjima u farmaciji. Naročito se govori o klasifikaciji brojnih tipova dizajna i njihovim mogućnostima za racionalizaciju različitih faza tokom procesa razvoja HPLC metode, kao što su izbor najuticajnijih faktora, optimizacija faktora i procena robusnosti metode. Dodatno, sumirana je primena DOE kao sastavnog dela koncepta ugradnje kvaliteta u proizvod u domenu razvoja analitičkih metoda (AQbD) zasnovanih na HPLC tehnici. Takođe su prikazana i nedavna dostignuća u primeni DOE u razvoju LC metoda koje su pogodne za ispitivanje stabilnosti lekova, kao i LC-MS metoda. U budućoj perspektivi, preporučeno je izvođenje ispitivanja kvantitativnog odnosa između strukture i retencionog ponašanja (QSRR) analita u HPLC sistemu na osnovu podataka dobijenih primenom DOE.
PB - Beograd : Savez farmaceutskih udruženja Srbije
T2 - Arhiv za farmaciju
T1 - Experimental design in HPLC separation of pharmaceuticals
T1 - Primena eksperimentalnog dizajna za razdvajanje lekova HPLC metodom
VL - 71
IS - 4
SP - 279
EP - 301
DO - 10.5937/arhfarm71-32480
ER -
@article{
author = "Stojanović, Jevrem and Krmar, Jovana and Protić, Ana and Svrkota, Bojana and Đajić, Nevena and Otašević, Biljana",
year = "2021",
abstract = "Design of Experiments (DoE) is an indispensable tool in contemporary drug analysis as it
simultaneously balances a number of chromatographic parameters to ensure optimal separation
in High Pressure Liquid Chromatography (HPLC). This manuscript briefly outlines the theoretical
background of the DoE and provides step-by-step instruction for its implementation in HPLC
pharmaceutical practice. It particularly discusses the classification of various design types and
their possibilities to rationalize the different stages of HPLC method development workflow, such
as the selection of the most influential factors, factors optimization and assessment of the method
robustness. Additionally, the application of the DoE-based Analytical Quality by Design (AQbD)
concept in the LC method development has been summarized. Recent achievements in the use of
DoE in the development of stability-indicating LC and hyphenated LC-MS methods have also
been briefly reported. Performing of Quantitative structure retention relationship (QSRR) study
enhanced with DoE-based data collection was recomended as a future perspective in description
of retention in HPLC system., Dizajn eksperimenata (DoE) je nezaobilazan alat u savremenoj analizi lekova budući da istovremeno balansira niz hromatografskih parametara kako bi se osiguralo optimalno razdvajanje u tečnoj hromatografiji pod visokim pritiskom (HPLC). Prikazana je teorijska osnova DOE i data su detaljna uputstva za njegovu primenu u HPLC ispitivanjima u farmaciji. Naročito se govori o klasifikaciji brojnih tipova dizajna i njihovim mogućnostima za racionalizaciju različitih faza tokom procesa razvoja HPLC metode, kao što su izbor najuticajnijih faktora, optimizacija faktora i procena robusnosti metode. Dodatno, sumirana je primena DOE kao sastavnog dela koncepta ugradnje kvaliteta u proizvod u domenu razvoja analitičkih metoda (AQbD) zasnovanih na HPLC tehnici. Takođe su prikazana i nedavna dostignuća u primeni DOE u razvoju LC metoda koje su pogodne za ispitivanje stabilnosti lekova, kao i LC-MS metoda. U budućoj perspektivi, preporučeno je izvođenje ispitivanja kvantitativnog odnosa između strukture i retencionog ponašanja (QSRR) analita u HPLC sistemu na osnovu podataka dobijenih primenom DOE.",
publisher = "Beograd : Savez farmaceutskih udruženja Srbije",
journal = "Arhiv za farmaciju",
title = "Experimental design in HPLC separation of pharmaceuticals, Primena eksperimentalnog dizajna za razdvajanje lekova HPLC metodom",
volume = "71",
number = "4",
pages = "279-301",
doi = "10.5937/arhfarm71-32480"
}
Stojanović, J., Krmar, J., Protić, A., Svrkota, B., Đajić, N.,& Otašević, B.. (2021). Experimental design in HPLC separation of pharmaceuticals. in Arhiv za farmaciju
Beograd : Savez farmaceutskih udruženja Srbije., 71(4), 279-301.
https://doi.org/10.5937/arhfarm71-32480
Stojanović J, Krmar J, Protić A, Svrkota B, Đajić N, Otašević B. Experimental design in HPLC separation of pharmaceuticals. in Arhiv za farmaciju. 2021;71(4):279-301.
doi:10.5937/arhfarm71-32480 .
Stojanović, Jevrem, Krmar, Jovana, Protić, Ana, Svrkota, Bojana, Đajić, Nevena, Otašević, Biljana, "Experimental design in HPLC separation of pharmaceuticals" in Arhiv za farmaciju, 71, no. 4 (2021):279-301,
https://doi.org/10.5937/arhfarm71-32480 . .
