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Optimization of Extraction Methods for Determination of Phosphodiesterase-5 (PDE5) Inhibitors in Premix Coffee (Pengoptimuman Kaedah Pengekstrakan bagi Penentuan Perencat
Fosfodiesterase-5
(PDE5) dalam Kopi Pracampuran)
Zailina binti Abdul Majid*
National Public Health Laboratory, Ministry of
Health, Lot 1853, Kg. Melayu, 47000 Sg. Buloh, Selangor, Malaysia
Aminah Abdullah & Mohd Ambar Yarmo
School of Chemical Science and Food Technology, Faculty
of Science and Technology
Universiti Kebangsaan Malaysia, 43600 Bangi,
Selangor, Malaysia
Diserahkan: 21 Februari 2012 / Diterima: 9 Oktober
2012
ABSTRACT
An efficient analytical technique capable of analyzing three most
common phosphodiesterase-5 (PDE5) inhibitors (vardenafil,
sildenafil and tadalafil) simultaneously in premix coffee was developed. Sample
extractions using either acetonitrile or methanol with two different extraction
techniques (with and without evaporation steps) were evaluated. Identification
and quantitation was conducted by high performance liquid chromatography with
photo-diode-array (HPLC-DAD) at different wavelengths;
230 nm, 245 nm and 290 nm; and by time of flight mass spectrometry (LC-MS-TOF).
Extraction with acetonitrile (without evaporation with nitrogen) showed
recovery ranging from 105% to 113% (± <10%) for HPLC-DAD at
245 nm and 93% to 102% (± <2.5%) for LC-MS-TOF. Chromatogram
separation was best achieved with mobile phase consisted of water (0.1% formic
acid) and acetonitrile (0.1% formic acid) with gradient elution within 20 min.
Thus, the results indicated that extraction using acetonitrile without
evaporation step was the most efficient technique for determination of PDE5
inhibitors in premix coffee.
Keywords: HPLC-DAD; LC-MS-TOF;
optimization; PDE5 inhibitors; premix coffee
ABSTRAK
Satu kaedah pengekstrakan yang ringkas dan cekap
telah berjaya dibangunkan untuk mengesan kehadiran perencat fosfodiesterase-5 (PDE5)
iaitu vardenafil, sildenafil dan tadalafil dalam produk kopi pracampuran. Pengekstrakan sampel
menggunakan asetonitril atau metanol dengan dua kaedah pengekstrakan (melalui
dan tanpa melalui penyejatan bernitrogen) dinilai. Penentuan dan
kuantifikasi sebatian adalah menggunakan kromatografi cecair prestasi tinggi (HPLC)
dengan pengesan susunan diod (DAD) pada panjang gelombang 230
nm, 245 nm dan 290 nm serta kromatografi cecair spektrometri jisim masa
penerbangan (LC-MS-TOF). Pengekstrakan sampel menggunakan asetonitril
(tanpa melalui penyejatan bernitrogen) menunjukkan peratusan perolehan semula
antara 105% hingga 113% (± <10%) dengan HPLC-DAD pada
panjang gelombang 245 nm dan 93% hingga 102% (± <2.5%) dengan LC-MS-TOF.
Pemisahan kromatogram paling baik diperoleh dengan kombinasi fasa bergerak air
(0.1% asid formik) dan asetonitril (0.1% asid formik) dengan kecerunan elusi
dalam tempoh 20 min. Ini membuktikan kaedah pengekstrakan sampel menggunakan
asetonitril tanpa langkah penyejatan bernitrogen merupakan teknik yang paling
cekap dalam menentukan perencat PDE5 dalam produk kopi
pracampuran.
Kata kunci: HPLC-DAD;
kopi pracampuran; LC-MS-TOF;
pengoptimuman; perencat PDE5
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*Pengarang untuk surat-menyurat; email: zailina.am@moh.gov.my
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