Malaysian Journal of Analytical Sciences Vol 18 No 3 (2014): 491 - 506

 

 

 

FOUR SPECTROPHOTOMETRIC METHODS FOR SIMULTANEOUS DETERMINATION OF CARBAMAZEPINE AND LAMOTRIGINE IN BINARY MIXTURES AND URINE SAMPLES

 

(Penentuan Serentak Karbamazapin dan Lamotrigin Di Dalam Campuran Perduaan Dan Sampel Urin Melalui Empat Kaedah Spektrofotometrik)

 

Fadhil M. Najib^*, Muhammad S. Mustafa

 

Chemistry Department,
Faculty of Science and Science Education,

Sulaimani University, Kurdistan Region, Iraq

 

*Corresponding author: fadhil.najib@yahoo.com

 

 

Abstract

In this work four different UV-spectrophotometric methods are described for simultaneous determination of antiepileptic drugs; carbamazepine (CBZ) and lamotrigine (LMT) in binary synthetic mixtures and urine samples without separation. First method was by solving the two simultaneous equations (SEQ) based on total absorbance according to Beer’s law.  Second was Dual wavelength (DWSP) method; Absorbance difference between 304 and 313 nm was measureable for CBZ but  was zero for LMT. Likewise the absorbance difference between 282 and 290 nm was significant for LMT, and zero for CBZ. Third involved the use of zero- crossing first derivative method (ZCDSP) using the amplitudes at 308.9 and 286.6 nm for CBZ and LMT respectively. Ratio Derivative Spectrophotometry (RDSP) was the last.  Here, the absorbance at different concentrations of CBZ or LMT, was divided, wavelength by wavelength, by the absorbance of a divisor, which was LMT standard for the analyte CBZ, and vice versa for LMT, (Divisor=2.0µg.mL^-1) in both cases. The amplitude of the derivative ratio spectra at 290 nm with wavelength interval (Δλ=6.0nm) and 328 nm (Δλ=4.0 nm) were selected for the determination of CBZ and LMT respectively.  CBZ and LMT were simultaneously determined in synthetic mixtures and urine samples by the four methods giving good linearity, r² ranged between 0.9990 - 0.9997. Detection Limit (D.L) was mostly less than 0.4µg.mL^-1,while in case of ZCDSP and RDSP were between 0.01-0.2 µg.mL^-1  with wider linearity range (1-50 for CBZ and 1 - 80µg.mL^{- 1} for LMT). A slightly lower sensitivity was observed when suppressing solution for urine analysis was used to remove interferences. The recoveries of CBZ and LMT in samples of urine of a healthy person spiked with the drugs and using urine of a healthy person as a blank were, in most cases, around (101.0% - 103.33%) and (98.33% - 102.16%) with RSD 3.61 and 3.63% for CBZ and LMT respectively. The recoveries using suppressing solution were (101.66% - 105.41%) and (94.56% - 101.0%) with RSD 2.43 and 3.62% for CBZ and LMT respectively. Statistical comparison of the results with the mixture of standard solutions using F, and t-tests showed no significant differences between each of the four methods at 95% C.L. The proposed methods were successfully applied for the determination of CBZ and LMT in binary mixtures and urine samples.

 

Keywords: dual wave length, zero crossing derivative, ratio derivative spectrophotometry, tegretol and lamotigine determination

 

Abstrak

Dalam kajian ini empat kaedah spektrofotometri UV yang berbeza dijelaskan terhadap penentuan serentak dadah antiepilepsi; karbamazepin (CBZ) dan lamotrigin (LMT) dalam campuran sintetik perduaan dan sampel urin tanpa pemisahan. Kaedah pertama adalah dengan menyelesaikan dua persamaan serentak (SEQ) berdasarkan jumlah serapan menurut hukum Beer. Kedua adalah kaedah panjang gelombang dual (DWSP); Perbezaan serapan diukur antara 304 dan 313 nm terhadap CBZ manakala sifar bagi LMT. Begitu juga perbezaan serapan antara 282 dan 290 nm adalah penting untuk LMT dan set sifar untuk CBZ. Kaedah ketiga melibatkan penggunaan kaedah lintasan sifar terbitan pertama (ZCDSP) pada amplitud masing – masing 308.9 dan 286.6 nm untuk CBZ dan LMT. Kaedah spektrofotometri nisbah terbitan (RDSP) adalah yang terakhir. Serapan pada kepekatan yang berbeza CBZ atau LMT mengikut panjang gelombang, oleh serapan pembahagi, dimana larutan LMT adalah piawai untuk analit CBZ analit, dan sebaliknya. (Kepekatan Pembahagi = 2.0μg.mL^-1) dalam kedua-dua kes. Amplitud nisbah spektrum terbitan pada 290 nm dengan selang jarak gelombang (Δλ = 6.0nm) dan 328 nm (Δλ = 4.0 nm) masing – masing telah dipilih untuk penentuan CBZ dan LMT. CBZ dan LMT telah ditentukan secara serentak di dalam campuran sintetik perduaan dan sampel urin oleh kesemua kaedah memberi kelinearan baik, r2 adalah antara 0.9990 - 0.9997. Had pengesanan adalah kurang daripada 0.4μg.mL^-1, manakala bagi kaedah lintasan sifar terbitan pertama dan spektrofotometri nisbah terbitan adalah di antara 0.01 – 0.2 μg.mL^-1 dengan julat kelinearan lebih besar (1-50 bagi CBZ dan 1 - 80μg.mL^-1 untuk LMT). Nilai sensitiviti diperhatikan lebih rendah apabila larutan tekanan digunakan terhadap analisis sampel urin untuk menghilangkan gangguan. Perolehan semula di dalam sampel urin bagi orang yang sihat yang dipaku bersama dadah CBZ dan LMT dan larutan pengosong dalam kebanyakan kes didapati  pada julat (101.0% - 103.33%) dan (98.33% - 102.16%) dengan RSD 3.61 dan 3.63% masing – masing terhadap CBZ dan LMT. Perolehan semula menggunakan larutan tekanan adalah (101.66% - 105.41%) dan (94,56% - 101.0%) dengan RSD 2.43 dan 3.62% masing – masing terhadap CBZ dan LMT. Perbandingan statistik hasil kajian menggunakan ujian F dan ujian-t terhadap larutan piawai menunjukkan tidak ada perbezaan yang signifikan antara setiap satu daripada empat kaedah pada 95%. Kaedah yang dicadangkan telah berjaya diggunakan terhadap penentuan campuran perduaan CBZ dan LMT dan sampel urin.

 

Kata kunci: panjang gelombang dual, kaedah lintasan sifar terbitan pertama, kaedah spektrofotometri nisbah terbitan, penentuan tegretol dan lamotigine

 

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