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Journal of Organic & Inorganic Chemistry
ISSN 2472-1123
2
n d
E d i t i o n o f E u r o S c i C o n C o n f e r e n c e o n
Chemistry
F e b r u a r y 1 9 - 2 0 , 2 0 1 9
P r a g u e , C z e c h R e p u b l i c
Chemistry 2019
T
he aim of this study was to validate direct swab and indirect rinse sampling procedures and demonstrate the applicability of
developed HPLC method for quantitative estimation of residues of active pharmaceutical ingredient-alprazolam residues as
a high potent and practically insoluble compound in water in cleaning control samples collected from pharmaceutical equipment
surfaces after manufacturing of alprazolam 1 mg uncoated tablets. The swab and rinse sampling procedures were developed
in order to obtain a suitable and good recovery (> 90%). The sampling procedures were qualified in respect to the validation
parameters. The known amounts of alprazolam at three different concentration levels are spiked onto representative surfaces,
which are disinfected and cleaned, then dried, sampled using swabbing and rinsing and analysed using the validated HPLC
method. Additionally, the robustness of sampling procedures was assessed. For swab sampling the surface (sampling area-25
cm
2
) was successively wiped with one micro polyester swab (3×2.5×10 mm) moistened with diluent methanol. The influence of
swab material on quantitative determination of alprazolam was checked as well. The method for quantitative determination of
alprazolam residues was developed using LC system Ag 1260 Infinity and Prodigy C8(2) 250×4.0 mm, 5 µm column with a mobile
phase: a mixture of methanol, phosphate buffer pH 3.0 and acetonitrile (10:45:45 v/v); the flow rate-1.4 mL/min; the detector
wavelength-220 nm; the injection volume-20 μL; the column temperature-300 °C. The method was validated with respect to
robustness, system suitability test, specificity, linearity-range, accuracy, precision (intra-day and inter day), limit of detection
(LOD) and quantitation (LOQ). The stability of alprazolam sample solutions and 0.45 µm membrane filter compatibility were
studied as well. These studies were performed in accordance with established ICH Q2 guideline and USP requirements. The
calibration curve is linear (r
2
=1.00000) over a wide concentration range of 0.0075-10 µg/mL; LOQ-0.0075 µg/mL and LOD-0.005
µg/mL. The method can be applied to determine quantitatively alprazolam residues in test solutions with very low concentrations
below the acceptable concentration of the cross-contamination limit.
rubashvili@yahoo.frDevelopment and validation of sampling procedures
and quantitative determination HPLC methods of
active pharmaceutical ingredient-alprazolam
residues on pharmaceutical technological equipment
Imeda Rubashvili
Petre Melikishvili Institute of Physical and Organic Chemistry-Ivane Javakhishvili Tbilisi State Uni-
versity, USA
J Org Inorg Chem 2019, Volume: 5
DOI: 10.21767/2472-1123-C1-021