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Sains Malaysiana 42(2)(2013):
135–142
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
Received: 21 February 2012 / Accepted: 9 October
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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*Corresponding author; email: zailina.am@moh.gov.my
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