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"Gabapentin, an anticonvulsant drug is used in the treatment of epilepsy, which has small dose therapeutic in blood plasma. Therapeutic drug monitoring (TDM) needs sensitive and specific analytical method.The aim of this study was to obtaine optimized method for analytical gabapentine in plasma (in vitro) with High Performance Liquid Chromatography - fluorescence and validation the method. The method involves derivatization of the primary amine group of gabapentin with dansyl chloride produce flurescence agent and could be analyzed with high performance liquid chromatography-fluorescence.In this research was used column Lichrosphere C18 ,10 μm, 250 x 10 μm, reverse phase with mobile phase 50 mmol/L sodium dihydrogen phosphate in 50 % acetonitrile. Flow rate of 1.7 mL/minutes, and fluorometric detection ( excitation and emission wavelength ; 318 nm and 510 nm ). For the range concentration of 0.1 ? 10 μg/mL have correlation coefficients of the calibration curves (r) is 0.9982 with a lower limit of quantification of gabapentin in 30 ng/mL. The results of validation method fulfilled for the given criterias."

"Metode kromatografi cair kinerja tinggi yang sederhana dan reprodusibel telahdikembangkan untuk penentuan kadar sulfametoksazol (SMX) dan trimetoprim(TMP) secara simultan di dalam tablet dan plasma manusia secara in vitro. Sistemkromatografi terdiri dari kolom C18 (250 mm × 4.6 mm, 5 μm) dengan fase gerakasetonitril-air-trietilamin (20:80:0,1 v/v), pH 5,9 ± 0,1 diatur dengan NaOH 0,2 Ndan asam asetat 1%. Larutan dideteksi pada panjang gelombang UV 240 nm dananalisis dilakukan pada laju alir 1,0 mL/menit suhu ruang. Sebagai baku dalamdigunakan sulfadimidin. Pada validasi tablet, metode dinyatakan linear dengannilai koefisien korelasi (r) untuk trimetoprim dan sulfametoksazol berturut-turut0,9994 dan 0,9996; presisi dengan nilai koefisien variasi (KV) 0,85% dan 0,98%;serta akurat dengan nilai perolehan kembali untuk 3 konsentrasi sebesar 98% -102%. Proses ekstraksi plasma dilakukan dengan metode pengendapan proteinmenggunakan asetonitril kemudian divortex selama 40 detik dan disentrifugasipada kecepatan 12500 rpm selama 15 menit. Pada validasi plasma, nilai perolehankembali rata-rata untuk trimetoprim dan sulfametoksazol berturut-turut 94,95%dan 86,87% serta nilai LLOQ berturut-turut 0,15 μg/mL dan 0,75 μg/mL. Metodeini juga memenuhi kriteria akurasi dan presisi intra hari dan antar hari selama 5hari dengan % diff tidak melampaui ± 20% pada LLOQ dan ± 15% padakonsentrasi selain LLOQ. Pada uji stabilitas, kotrimoksazol dalam plasmadinyatakan tetap stabil selama 30 hari."

"Metode kromatografi cair kinerja tinggi (KCKT) dengan detektor fluoresensi untuk menganalisis ofloksasin dalam plasma telah dikembangkan. Tujuan dari penelitian ini adalah memperoleh kondisi yang optimum untuk analisis ofloksasin dalam plasma in vitro dan melakukan validasi metode analisis tersebut. Kondisi kromatografi menggunakan kolom C18 dengan fase gerak asetonitril-larutan kalium dihidrogen fosfat 0,01 M (140:860; v/v) pH 3, kecepatan alir 1,0 ml/menit dan dideteksi dengan detektor fluoresensi pada panjang gelombang eksitasi 300 dan emisi 500 nm. Siprofloksasin digunakan sebagai baku dalam. Teknik penyiapan sampel dilakukan dengan cara pengendapan protein menggunakan asetonitril, kemudian supernatannya dipisahkan lalu diinjeksikan ke dalam kolom. Metode ini memberikan nilai linearitas pada rentang konsentrasi 1,0 -5,0 g/ml dengan nilai koefisien korelasi (r) 0,9998. Batas deteksi pada metode ini konsentrasi 0,102 g/ml dan batas kuantitasi 0,340 g/ml. Metode ini memberikan hasil uji perolehan kembali pada konsentrasi 1,02 g/ml adalah 90,668 0,2635 %, konsentrasi 3,06 g/ml adalah 92,932 0,6468 % dan konsentrasi 5,1 g/ml adalah 95,594 3.184 %.

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A high-performance liquid chromatographic method (HPLC) with fluorescence detector for analyses of ofloxacin in human plasma was developed. The aim of this research is to find out optimum condition of ofloxacin in human plasma with in vitro analysis using High Performance Liquid Chromatography (HPLC) and then validate the method. Condition of chromatography using C18 column with a mixture of acetonitril-0,01 M dihydrogenpotassium phosphate solution (140:860) pH 3 as mobile phase, at flow rate 1,0 ml/menit, with fluorimetric detection was performed at 300 nm for excitation and 500 nm for emission. Ciprofloxacin was used as an internal standard. The sampel preparation technique was protein precipitation with acetonitril, the supernatant was desperated and injected into C18 column. Linearity was established for range of concentration 1.0-5.0 g/ml with coefficient of correlation of 0.9998. The limit of detection (LOD) was identifiable and reproducible at 0.102 g/ml and the limit of quantitaion (LOQ) at 0.340 g/ml. This method has ofloxacin recovery was 90.668 0,2635 % for concentration 1.02 g/ml, 92,932 0,6468 % for concentration 3.06 g/ml, and 95,594 3.184 % for concentration 5.1 g/ml."

"[ABSTRAKAsaro valproat adalah satu dari banyak obat yang digunakan sebagai antiepilepsi dan memiliki banyak efek samping, sehingga direkomendasikan untuk menentukan konsentrasinya di dalam plasma. Penelitian ini bertujuan untuk memvalidasi metode analisis asam valproat setelah diderivatisasi dengan 2,4-dibromoasetofenon di dalam plasma in-vitro dan in-vivo, menggunakan kromatografi cair kinerja tinggi- Photo Diode Array.Asam valproat dan asam nonanoat sebagai baku dalam diekstraksi dari plasma dengan etil asetat. Supematan yang diperoleh dinetralkan dan diuapkan, kemudian residu kering direkonstitusi dengan larutan penderivat-katalis dalam asetonitril kemudian diderivatisasi pada suhu 75°C selama 25 menit. Pemisahan dilakukan menggunakan kolom C18 Sunfire ® (250 mm x 4,6, 5 Jlm) dengan elusi isokratik menggunakan fase gerak asetonitril-air (73 :27). Pengukuran dilakukan pada panjang gelombang 294 nm dengan kecepatan alir 1,5 mL/menit. Metode ini valid berdasarkan hasil LOQ 4,75 flg/mL, perolehan kembali relatif konsentrasi rendah, sedang dan tinggi berturut-turut 100,67%, 99,78%, dan 93,16%. Koefisien variasi intra dan inter day dan persen penyimpangan (SD) dari metode ini masuk dalam kriteria penerimaan, yaitu dibawah ± 15%. Kurva kalibrasi linier dalam plasma in-vitro (Y = 0,0123 + 0,0085X) pada konsentrasi 4,75-237,75 Jlg/mL dengan nilai r =0,9999. Metode yang dihasilkan dapat diaplikasikan untuk menetapkan kadar asam valproat dalam plasma setelah pemberian secara oral tablet natrium divalproat 500 mg.

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ABSTRACTValproic acid is one of mostly used antiepileptic drug which have side effects, so it is highly recommended to evaluate its plasma concentration The aim of the research was to validate a method for the determination valproic acid in plasma in-vitro and in-vivo after derivatization with 2,4-dibromasetofenon using high performance liquid chromatography-photo diode array. Valproic acid and internal standard nonanoic acid were extracted from plasma sample with ethyl acetate. Then supematan was neutralizatied and evaporated. dried residue reconsituted in derivate-catalyst solution then derivatized at 75°C for25 minutes. The resulting derivatives were separated on a Sunfire C18 (250 mm x 4.6, 5 Jlm) reverse phase column with acetonitrile-water (73:27) asmobile phase, were detected at 294 nm and analysis were tun at flow rate 1.5 mL/minute. The calibration curve in plasma in-vitro ( Y =0.0123 + 0.0085 x) presented good linier (r = 0.9999) between 4.75-237.75 Jlg/mL with LLOQ4.75 Jlg/mL. The mean of relative recovery at low concentration, middle concentration and high concentration are 100.67%, 99.78%, and 93.16 %, respectively. Intra- and inter- day coefficient of variation and percent error value of the assay method were all acceptable range ± 15%. The presented method was might be applied to the determine of the valproic acid concentration in plasma after oral administration of 500 mg sodium divalproate., Valproic acid is one of mostly used antiepileptic drug which have side effects, so it is highly recommended to evaluate its plasma concentration The aim of the research was to validate a method for the determination valproic acid in plasma in-vitro and in-vivo after derivatization with 2,4-dibromasetofenon using high performance liquid chromatography-photo diode array. Valproic acid and internal standard nonanoic acid were extracted from plasma sample with ethyl acetate. Then supematan was neutralizatied and evaporated. dried residue reconsituted in derivate-catalyst solution then derivatized at 75°C for25 minutes. The resulting derivatives were separated on a Sunfire C18 (250 mm x 4.6, 5 Jlm) reverse phase column with acetonitrile-water (73:27) asmobile phase, were detected at 294 nm and analysis were tun at flow rate 1.5 mL/minute. The calibration curve in plasma in-vitro ( Y =0.0123 + 0.0085 x) presented good linier (r = 0.9999) between 4.75-237.75 Jlg/mL with LLOQ4.75 Jlg/mL. The mean of relative recovery at low concentration, middle concentration and high concentration are 100.67%, 99.78%, and 93.16 %, respectively. Intra- and inter- day coefficient of variation and percent error value of the assay method were all acceptable range ± 15%. The presented method was might be applied to the determine of the valproic acid concentration in plasma after oral administration of 500 mg sodium divalproate.]"

"Siklofosfamida adalah obat antineoplastik yang sering diberikan dalam regimen kemoterapi dosis tinggi. Adanya toksisitas tinggi dari regimen tersebut, maka diperlukan analisis siklofosfamida dalam plasma untuk memonitor kadarnya. Pada penelitian ini, telah dikembangkan metode kromatografi cair kinerja tinggi yang sederhana dan reprodusibel untuk penentuan kadar siklofosfamida dalam plasma manusia. Sistem kromatografi terdiri dari kolom Shimpack® C18 (250 × 4,6 mm, 5 μm) dengan fase gerak asetonitril-KH2PO4 10 mM mengandung 0,5% trietilamin (37 : 63 v/v) dengan pH 6,5 untuk analisis di dalam plasma secara in vitro, dengan laju alir 1,0 mL/menit. Sampel dideteksi pada panjang gelombang 200 nm. Pada penelitian ini juga dilakukan pemilihan baku dalam yang sesuai yaitu irbesartan dan parasetamol. Proses ekstraksi plasma dilakukan dengan metode pengendapan protein menggunakan asetonitril dan semua kriteria memenuhi persyaratan yang diberikan oleh (EMEA, 2011). Metode valid pada rentang 0,204 μg/ml ? 20,0 μg/ml diperoleh nilai koefisien korelasi (r) 0,9995 . Metode ini memenuhi kriteria akurasi dengan %diff sebesar -14,64% - 14,91% serta presisi dengan koefisien variasi <9,6%.

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Cyclophosphamide is a antineoplastic prodrug are often administered in high-dose chemotherapy regimens. The high toxicities from this regimens, analytical method is required to determine the concentration of cyclophosphamide in human plasma. In this research, a simple and reproducible high-performance liquid chromatography method was developed for simultaneous determination of cyclophosphamide in human plasma. Chromatography was performed on a Shimpack® C18 column (250 × 4.6 mm, 5 μm) under isocratic elution with acetonitrile ? potassium dihydrogen phosphate buffer containing 0,5% triethylamine (37 : 63 v/v) pH 6,5 for analytical in human plasma, and the flow- rate was 1.0 ml/min. Detection was made at 200 nm. In this research, also has done the selection of the appropriate for internal standard are irbesartan and paracetamol. Plasma extraction was done by deproteination with acetonitrile and all the parameters were fulfilled the criteria that were given by (EMEA, 2011). The method was valid over the range of 0,204 ? 20 μg/ml get correlation coefficient (r) values 0.9995. The method was validated with accuracies of (% diff) -14,64% - 14,45 % and precision < 9,6%."

"Rabeprazol merupakan obat golongan penghambat pompa proton yang digunakan untuk pengobatan refluks gastroesophageal. Konsentrasinya sangat kecil dalam plasma sehingga diperlukan metode analisis yang sensitif, selektif, dan akurat. Pada penelitian ini, dilakukan optimasi dan validasi metode analisis rabeprazol dalam plasma in vitro menggunakan kromatografi cair kinerja tinggi UV-Vis dengan pantoprazol sebagai baku dalam. Pemisahan menggunakan kolom Kromasil® C18, 100-5, (4,6 × 250 mm, 5 μm) dengan fase gerak isokratik yang terdiri dari 50 mM natrium dihidrogen fosfat pH 7,2 - asetonitril (55:45, v/v). laju alir 0,5 mL/menit dan dideteksi pada panjang gelombang 294 nm. Waktu retensi rabeprazol dan pantoprazol adalah 8,7 dan 9,8 menit dengan total waktu analisis adalah 12 menit. Sampel plasma (500 μL) diekstraksi menggunakan dietil eter-diklorometan (90:10, v/v). Metode ini spesifik karena tidak adanya puncak pengganggu plasma pada waktu retensi analit dan baku dalam. Metode ini valid dan linear pada rentang konsentrasi 10,08 - 1008,00 ng/mL dengan LLOQ 10,0 ng/mL (n = 6, koefisien variasi (KV) = 3,16%). Nilai % diff dan koefisien variasi untuk akurasi dan presisi intra hari dan antar hari tidak lebih dari 15%. Nilai perolehan kembali absolut dari rabeprazol sebesar 76 - 87% (KV = 6,54%) dan baku dalam sebesar 74% (KV = 3,13%). Rabeprazol dalam plasma dinyatakan stabil selama minimal 1 bulan pada suhu -20°C dan -80°C, stabil selama minimal 12 jam pada suhu kamar. Rabeprazol dinyatakan stabil selama 3 siklus beku dan cair. Metode ini memenuhi kriteria penerimaan seperti pada pedoman USFDA dan bisa diaplikasikan untuk analisis rabeprazol dalam plasma in vivo.

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Rabeprazole is a proton-pump inhibitor, used in gastroesophageal reflux treatment. Its concentration is very small in human plasma, so it requires a sensitive, selective, and accurate method of analysis. In this study, carried out optimization and validation of rabeprazole analysis in human plasma using high performance liquid chromatography UV-Vis using pantoprazole as internal standard. Separation was performed on Kromasil® 100-5 C18, (4.6 × 250 mm, 5μm) column with an isocratic mobile phase composed of 50 mM sodium dihydrogen phosphate pH 7.2 - acetonitrile (55:45, v/v), flow rate at 0.5 mL/min and was detected at 294 nm. Retention time of rabeprazole and pantoprazole were 8.7 and 9.8 minutes and total analytical run time was 12 minutes. Plasma sample (500 μL) was extracted with diethyl eter - dichloromethane (90:10, v/v).

The method was specific as there were no interfering peaks of human plasma eluting at the retention times of the rabeprazole and the internal standard. The method was valid and linear within the concentration ranges of 10.08-1008.00 ng/mL with LLOQ 10,0 ng/mL (n = 6, coefficient variation (CV) = 3.16%). Intra-day and inter-day accuracy and precision was not more than 15% in both % diff and coefficient of variation. Absolute recovery were 76-87% (CV = 6.54%) for rabeprazole and 74% (CV = 3.13%) for internal standard. Rabeprazole was stable in human plasma for at least 1 month at -20°C and -80°C, and for 12 h at room temperature. Rabeprazole were stable to three freeze thaw cycles. This method also fulfil the acceptance criteria following USFDA guidelines and suitable to be applied for analysis of rabeprazole in human plasma."