TY - JOUR
T1 - Rilpivirine and Dolutegravir Simultaneously Measured via RP-HPLC-PDA with Box–Behnken Design Application
T2 - A Study of Forced Degradation under Various Conditions
AU - Wahab, Shadma
AU - Khalid, Mohammad
AU - Ahmad, Sarfaraz
AU - Sweilam, Sherouk Hussein
N1 - Publisher Copyright:
© 2023 by the authors.
PY - 2023/3
Y1 - 2023/3
N2 - Simultaneous estimation of rilpivirine (RLVN) and dolutegravir (DTGR) in bulk and tablet dosage forms via RP-HPLC-PDA with a Box–Behnken design (BBD) has been performed in this study to develop a fast, precise, timely and cost-saving method for estimating RLVN and DTGR in bulk and tablet dosage forms. The chromatographic conditions were optimized via the BBD, and the developed method was validated according to the ICH guidelines. Additionally, forced degradation studies were also conducted. RLVN and DTGR peaks were observed at retention times of 2.167 and 2.716 min, respectively, in a 6-min runtime. Kromasil 150 mm× 4.6 mm, 5 µm C 18 column was used. The flow rate of the mobile phase was 1.0 mL/min at a temperature of 30 °C. The mobile phase composition was a 0.1% OPA buffer and acetonitrile (ACN) in a 60:40 ratio. Elutes were measured at 260 nm (max) after being injected in a sample volume of 10 µL. The assay result of the marketed tablet was 99.19% and 99.09% for RLVN and DTGR, respectively. The results of forced degradation studies in different chemical environments conditions such as acid, base, dry heat, photo-stability, neutral, and oxidation conditions were observed for RLVN (5.96, 4.79, 3.27, 2.36, 0.99, and 4.35 in percentage degradation) and DTGR (5.67, 4.44, 4.09, 1.81, 0.43, and 4.28 in percentage degradation). The results of the validation parameters were within an acceptable range. The newly formed RP-HPLC-PDA method is novel, fast, precise, time-saving, and cost-effective.
AB - Simultaneous estimation of rilpivirine (RLVN) and dolutegravir (DTGR) in bulk and tablet dosage forms via RP-HPLC-PDA with a Box–Behnken design (BBD) has been performed in this study to develop a fast, precise, timely and cost-saving method for estimating RLVN and DTGR in bulk and tablet dosage forms. The chromatographic conditions were optimized via the BBD, and the developed method was validated according to the ICH guidelines. Additionally, forced degradation studies were also conducted. RLVN and DTGR peaks were observed at retention times of 2.167 and 2.716 min, respectively, in a 6-min runtime. Kromasil 150 mm× 4.6 mm, 5 µm C 18 column was used. The flow rate of the mobile phase was 1.0 mL/min at a temperature of 30 °C. The mobile phase composition was a 0.1% OPA buffer and acetonitrile (ACN) in a 60:40 ratio. Elutes were measured at 260 nm (max) after being injected in a sample volume of 10 µL. The assay result of the marketed tablet was 99.19% and 99.09% for RLVN and DTGR, respectively. The results of forced degradation studies in different chemical environments conditions such as acid, base, dry heat, photo-stability, neutral, and oxidation conditions were observed for RLVN (5.96, 4.79, 3.27, 2.36, 0.99, and 4.35 in percentage degradation) and DTGR (5.67, 4.44, 4.09, 1.81, 0.43, and 4.28 in percentage degradation). The results of the validation parameters were within an acceptable range. The newly formed RP-HPLC-PDA method is novel, fast, precise, time-saving, and cost-effective.
KW - Box–Behnken design
KW - cost-effective
KW - degradation studies
KW - ICH guidelines
KW - PDA detector
KW - RP-HPLC
UR - http://www.scopus.com/inward/record.url?scp=85151157750&partnerID=8YFLogxK
U2 - 10.3390/separations10030185
DO - 10.3390/separations10030185
M3 - Article
AN - SCOPUS:85151157750
SN - 2297-8739
VL - 10
JO - Separations
JF - Separations
IS - 3
M1 - 185
ER -