LC method
development and analyses were performed on Acquity UPLC H-Class systems
(Waters, Millford, MA, USA) equipped with a quaternary solvent manager
(QSM), sample manager with a flow-through needle (SM-FTN), and either
photodiode array (PDA) or tunable ultraviolet (TUV) optical detector.
LC systems were equipped with Empower 3 data software (Waters, Millford,
MA, USA).
Chromatography columns used during AQbD development
were as listed: XBridge C8, 3.5 μm, 150 mm × 4.6 mm; XBridge
C18, 3.5 μm, 150 mm × 4.6 mm; Acquity UPLC BEH Phenyl,
1.7 μm, 150 mm × 2.1 mm and Acquity UPLC HSS T3, 1.8 μm,
150 mm × 2.1 mm (Waters, Millford, MA, USA). AQbD was done with
S-Matrix Fusion QbD Pro 9.8 (S-Matrix, Eureka, CA, USA). Cabotegravir
drug substance and its impurities were weighed within a ventilated
balance enclosure OK 15 (Iskra Pio, Šentjernej, Slovenia) on
either an XP4002S precision balance, XP205 DeltaRange analytical balance,
AX205 DeltaRange analytical balance, or MX5 microbalance (Mettler
Toledo, Columbus, OH, USA). pH was measured using a SevenMulti pH
meter (Mettler Toledo, Columbus, OH, USA). Pipettes used were Handystep
electronic repetitive pipettes (Brand, Wertheim, Germany). Ultrasonic
baths used were Branson 8510 (Emerson Electric, St. Louis, MO, USA),
Sonic 10 and Sonic 20 (Iskra Pio, Šentjernej, Slovenia). Stress
testing was done in a BF 720 standard incubator (Binder, Tuttlingen,
Germany).
development and analyses were performed on Acquity UPLC H-Class systems
(Waters, Millford, MA, USA) equipped with a quaternary solvent manager
(QSM), sample manager with a flow-through needle (SM-FTN), and either
photodiode array (PDA) or tunable ultraviolet (TUV) optical detector.
LC systems were equipped with Empower 3 data software (Waters, Millford,
MA, USA).
Chromatography columns used during AQbD development
were as listed: XBridge C8, 3.5 μm, 150 mm × 4.6 mm; XBridge
C18, 3.5 μm, 150 mm × 4.6 mm; Acquity UPLC BEH Phenyl,
1.7 μm, 150 mm × 2.1 mm and Acquity UPLC HSS T3, 1.8 μm,
150 mm × 2.1 mm (Waters, Millford, MA, USA). AQbD was done with
S-Matrix Fusion QbD Pro 9.8 (S-Matrix, Eureka, CA, USA). Cabotegravir
drug substance and its impurities were weighed within a ventilated
balance enclosure OK 15 (Iskra Pio, Šentjernej, Slovenia) on
either an XP4002S precision balance, XP205 DeltaRange analytical balance,
AX205 DeltaRange analytical balance, or MX5 microbalance (Mettler
Toledo, Columbus, OH, USA). pH was measured using a SevenMulti pH
meter (Mettler Toledo, Columbus, OH, USA). Pipettes used were Handystep
electronic repetitive pipettes (Brand, Wertheim, Germany). Ultrasonic
baths used were Branson 8510 (Emerson Electric, St. Louis, MO, USA),
Sonic 10 and Sonic 20 (Iskra Pio, Šentjernej, Slovenia). Stress
testing was done in a BF 720 standard incubator (Binder, Tuttlingen,
Germany).