A NEW INVESTIGATIONAL METHOD FOR QUANTIFICATION AND VALIDATION OF ANALYTICAL METHOD FOR CEFIXIME AND ERDOSTEINE BY UPLC WITH PHOTO DIODE ARRAY DETECTOR IN BULK AND FORMULATION. APPLICATION TO THE ESTIMATION OF PRODUCT TRACES

Specific and innovative method was developed and validated for the identification and quantification of cefixime and erdosteine in the bulk and formulation samples by UPLC with PDA detector.The analytical technique was with buffer (pH: 7.0): methanol, (65:35%, v/v) using the Sunfire C18, 5μ, 46mmX150mm analytical column with analysis time of six minutes. Flow of mobile phase through the column was 1.0 mL/min. Sample volume was 10 μL. Detection was carried at 254 nm in photo diode array detector. The retention times of cefixime and erdosteine were 2.012 min and 3.122 min., respectively. The curve indicates that correlation coefficient (r2) was superior by having the value 1.000 with linear range of 20.0 ng/mL-200.0 ng/mL for Cefixime and 30 ng/mL-300.0 ng/mL for erdosteine. The correlation coefficient (r2) for erdosteine found 1.000. The LoQ for cefixime and erdosteine was 20ng/mL and 30ng/mL respectively. The LOD for cefixime and erdosteine was 1.0 ng/mL and 1.5 ng/mL respectively. The developed method was applied for the bulk and formulation and equipement cleaning sample.

Optimasi Metode KCKT untuk Penetapan Kadar 4-Isobutilasetofenon dan 2-(4-Isobutirilfenil) Asam Propanoat dalam Tablet Ibuprofen

Pendahuluan: Ibuprofen (IBP) banyak digunakan sebagai obat anti piretik dan pereda nyeri, obat ini sensitif terhadap oksidasi dan suhu. Cemaran IBP yang keberadaannya dalam tablet harus memenuhi syarat uji batas adalah 4-isobutilasetofenon (IBP RC C) dan 2-(4-isobutirilfenil) asam propanoat (IBP RC J). Variasi matriks tablet seringkali membuat prosedur standar untuk analisis cemaran perlu dioptimasi karena dapat menyebabkan kinerja kromatografi yang tidak memenuhi syarat kompendia. Tujuan: Penelitian ini bertujuan untuk memperoleh kolom dan kondisi operasional KCKT yang selektif, efisien dan memenuhi persyaratan kompendia untuk pengujian IBP dan cemarannya. Metode: Penelitian ini dirancang untuk membandingkan kinerja kromatografi (resolusi, faktor ikutan dan jumlah lempeng teoritis) beberapa kolom KCKT C18 yang sesuai persyaratan United States Pharmacopoeia (USP) untuk penetapan cemaran organik dalam tablet ibuprofen. Instrumen KCKT yang digunakan adalah Shimadzu Prominence dengan detektor Photo Diode Array (PDA). Kondisi analisis optimum yang diperoleh diaplikasikan untuk analisis 3 macam sediaan tablet IBP. Hasil: Kondisi optimum diperoleh melalui kolom C18-C 4,6 x 250 mm, 5 µm, menggunakan fase gerak larutan asam kloroasetat 1% pH 3,0 : asetonitril (45:55, v/v), laju alir 1,5 mL/menit, suhu kolom ambient, detektor PDA 254 nm, volume injeksi 10 µL dengan waktu analisis 11 menit. Diperoleh puncak-puncak yang simetris dengan kinerja kromatografi yang memenuhi persyaratan USP. Kesimpulan: Metode yang telah dioptimasi berhasil diaplikasikan pada 3 sediaan tablet yang beredar di pasaran dan dapat digunakan untuk pengujian rutin dalam rangka pengawasan kualitas produk obat tablet ibuprofen.

Determining High-Intensity Sweeteners in White Spirits Using an Ultrahigh Performance Liquid Chromatograph with a Photo-Diode Array Detector and Charged Aerosol Detector

In China, white spirit is not only an alcoholic drink but also a cultural symbol. A novel and accurate method for simultaneously determining nine sweeteners (most authorized for use in China) in white spirits by ultrahigh performance liquid chromatography (UHPLC) with a photo-diode array detector (PDA) and charged aerosol detector (CAD) was developed. The sweeteners were acesulfame, alitame, aspartame, dulcin, neotame, neohesperidine dihydrochalcone, saccharin, sodium cyclamate, and sucralose. The sweeteners were separated within 16 min using a BEH C18 column and linear gradient-elution program. The optimized method allowed low concentrations (micrograms per gram) of sweeteners to be simultaneously detected. The CAD gave good linearities (correlation coefficients > 0.9936) for all analytes at concentrations of 0.5 to 50.0 μg/g. The limits of detection were 0.16 to 0.77 μg/g. Acesulfame, dulcin, neohesperidine dihydrochalcone, and saccharin were determined using the PDA detector, which gave correlation coefficients > 0.9994 and limits of detection of 0.16 to 0.22 μg/g. The recoveries were 95.1% to 104.9% and the relative standard deviations were 1.6% to 3.8%. The UHPLC-PDA-CAD method is more convenient and cheaper than LC-MS/MS methods. The method was successfully used in a major project called “Special Action against Counterfeit and Shoddy white spirits” and to monitor risks posed by white spirits in China.