Aplikasi Fourier Transform Infrared Spectrophotometry dengan Kemometrika dalam Penetapan Kadar Kreatin Monohidrat pada Sediaan Floating Tablet

Anas Ardiana Wati, Apt. Marlyn Dian Laksitorini, M.Sc. PhD.; Dr. apt. Agustina Ari Murti Budi Hastuti, S.Farm., M.Sc.

2023 | Skripsi | FARMASI

Kreatin sebagai zat ergogenik mampu meningkatkan performa olahraga serta

berkhasiat dalam terapi penyakit neurodegeneratif. Berbagai teknik spektroskopi

hingga kromatografi telah diterapkan dalam analisis kreatin. Namun demikian, metode

kromatografi memerlukan solvent organik dan waktu yang lebih lama. Pengembangan

spektroskopi FTIR kombinasi kemometrika dipilih dengan pertimbangan proses yang

mudah, cepat, serta pendekatan green chemistry untuk mencapai SDGs 13 yaitu

climate action. Penelitian ini bertujuan untuk penetapan kadar kreatin monohidrat pada

sediaan floating tablet. Target kedepannya, penelitian ini dapat diterapkan dalam

analisis rutin keseragaman kadar sediaan pada proses produksi di industri farmasi.

Pendekatan kemometrika dilakukan dengan kalibrasi multivariat model PCR

dan PLS yang didesain menggunakan bantuan software TQ Analyst. Validasi metode

dilakukan dengan mengevaluasi parameter statistik berupa R2, RMSEC, RMSEP,

RMSECV. Koleksi data spektra FTIR dilakukan dengan software Thermo Scientific™

OMNIC™ Series. Visualisasi dan pemprosesan spektra dikerjakan dengan software

Origin 2023.

Hasil pemindaian spektra dioptimasi melalui aspek pemilihan daerah

wavenumber serta jenis spektra. Berdasarkan hasil parameter validasi dipilih model

PLS pada spektra normal dengan wavenumber 1650-1350 cm-1. Model ini memberikan

hasil R2 untuk kalibrasi, validasi, dan cross-validation sebesar 0,9983; 0,9985; 0,9977

serta nilai RMSEC, RMSEP, dan RMSECV yaitu 1,74; 1,72; 2,07. Penerapan metode

ini untuk penetapan kadar kreatin monohidrat dalam sediaan floating tablet

memberikan hasil konsentrasi sebesar 99,99 ± 1,04% yang telah memenuhi

persyaratan kadar kreatin pada monografi USP 44.

Creatine as an ergogenic substance can improve sports performance and treat

neurodegenerative diseases. Various spectroscopic to chromatographic techniques

have been applied in the analysis of creatine. However, the chromatographic method

requires organic solvents and a longer time. The development of FTIR spectroscopy

with chemometrics was chosen because of an easy and fast process with consideration

of the green chemistry approach to achieve SDGs 13 (climate action). This study aims

to determine the levels of creatine monohydrate in floating tablet preparations. This

research can be applied in the routine analysis of dosage uniformity in production

processes in the pharmaceutical industry.

The chemometric approach was carried out by multivariate calibration of the

PCR and PLS models which were designed using TQ Analyst software. Method

validation was carried out by evaluating the statistical parameters of R2, RMSEC,

RMSEP, and RMSECV. FTIR spectral data collection was performed with the Thermo

Scientific™ OMNIC™ Series Software. Spectral visualization and processing were

done with the Origin 2023 software.

The results of the spectral scanning are optimized through the aspect of

wavenumber area and the type of spectra. Based on the results, the PLS model was

selected in the normal spectra with a wavenumber of 1650-1350 cm-1. This model gives

R2 results for calibration, validation, and cross-validation of 0.9983; 0.9985; 0.9977

and the RMSEC, RMSEP, and RMSECV values are 1.74; 1.72; 2.07. The application

of this method for determining creatine monohydrate content in floating tablet gave a

concentration of 99.99 ± 1.04% which met the requirements for creatine levels in USP

44 monograph.

Kata Kunci : kreatin monohidrat, floating tablet, FTIR, kemometrika