| Development and Validation of RP-HPLC Method for
Estimation of Methotrexate Drug Intercalated in Mg-Al
Layered Double Hydroxide Nanoparticles |
Arindam Basu,1 Sayantan Ray,2 Suman Saha2 and Jui Chakraborty2,*
Pages : 127-134
DOI : 10.1080/0371750X.2021.1904291 |
| Abstract |
| In the present study, pristine magnesium aluminium layered double hydroxide (Mg-Al
LDH, sample A) nanoparticles were synthesized by simple co-precipitation technique
followed by intercalation of methotrexate drug (MTX), their detailed physicochemical
characterization and development of RP-HPLC method for estimation of MTX
intercalated in Mg-Al LDH nanoparticles (sample B). The PXRD analysis showed the
basal spacing of 003 plane corresponding to sample A and sample B to be 8.63 Å and
11.39 Å, respectively. Particle size distributions were measured to be 56-75 nm
(D50=66.15 nm) in case of sample A and 75-100 nm (D50=87.41 nm) for sample B. Simple,
accurate RP-HPLC method was developed for estimation of the MTX drug from sample
B, on Agilent HPLC 1200 system with UV detector on L1 column. 0.02 M potassium
dihydrogen phosphate solution (pH 3.0) and acetonitrile (85:15 v/v) was used as mobile
phase in an isocratic elution mode at a flow rate of 1.0 mL/min at 35oC with a load of
10 L at 307 nm. The retention time for methotrexate was at 4.44 min. The method
was validated as per ICH Q2 (R1) guidelines. The method was found to be linear over
a concentration range of 10-100 g/mL.
[Keywords: Methotrexate drug, Mg-Al layered double hydroxide, RP-HPLC, Precision,
Accuracy] |
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