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Abstrak :
Asam 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. Supernatan yang diperoleh dinetralkan dan diuapkan, kemudian residu kering direkonstitusi dengan larutan penderivatkatalis dalam asetonitril kemudian diderivatisasi pada suhu 75ºC selama 25 menit. Pemisahan dilakukan menggunakan kolom C18 Sunfire ® (250 mm x 4,6, 5 µm) 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 µg/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 µg/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. ......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 supernatan was neutralizatied and evaporated. dried residue reconsituted in derivatecatalyst solution then derivatized at 75ºC for 25 minutes. The resulting derivatives were separated on a Sunfire C18 (250 mm x 4.6, 5 µm) reverse phase column with acetonitrile-water (73:27) as mobile phase , were detected at 294 nm and analysis were run 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 µg/mL with LLOQ 4.75 µg/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.

Abstrak :
[ABSTRAK
Asaro 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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ABSTRACT
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 for 25 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) as mobile 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 LLOQ 4.75 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 for 25 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) as mobile 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 LLOQ 4.75 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. ]

Abstrak :
ABSTRAK
Tamoksifen merupakan obat pilihan utama pengobatan kanker payudara pada wanita dengan reseptor estrogen positif ER , namun pada penggunaan jangka panjang selama 5-10 tahun berisiko menyebabkan secondary cancer berupa kanker endometrium. Penelitian ini bertujuan mendapatkan metode analisis yang sensitif, spesifik dan selektif yang mampu mengukur konsentrasi tamoksifen dan 4-hidroksitamoksifen di dalam plasma sebagai upaya memprediksi terjadinya secondary cancer dan mengetahui pengaruh pemberian fraksi aktif terhadap konsentrasi tamoksifen dan 4-hidroksitamoksifen menggunakan Kromatografi Cair Kinerja Ultra Tinggi-tandem Spektrometri Massa sesuai kriteria EMEA. Myrmecodia erinacea Becc. diekstraksi secara maserasi dengan etanol 80 untuk memperoleh ekstrak etanol 80 lalu difraksinasi dengan n-heksana, etil asetat dan butanol untuk mendapatkan fraksi aktif dan dilakukan identifikasi senyawa kimia. Dilakukan uji sitotoksik dan toksisitas akut terhadap fraksi aktif, lalu uji aktivitas kemopreventif menggunakan 30 tikus betina yang terbagi menjadi 6 kelompok perlakuan, yaitu diberikan tamoksifen 20 mg/kb bb KP , aqua destilata KKN , minyak jagung KN dan kelompok uji yang diberikan fraksi uji yang setara dengan kuersetin dosis 100, 200 dan 400 mg/kb bb. Tamoksifen 20 mg/kg bb diberikan pada seluruh kelompok kecuali KN dan KKN , setelah 30 menit diberikan fraksi uji pada kelompok perlakuan, selama 20 hari. Metode analisis yang dikembangkan sensitif, spesifik dan selektif pada LLOQ 2,0 ng/mL, rentang kurva kalibrasi 2,0-200,0 ng/mL,volume injek 1 L dengan waktu retensi tamoksifen, 4-hidroksitamoksifen dan propranolol HCl pada 1,59; 1,14; dan 1,09 menit. Fraksi aktif terpilih adalah etilasetat memiliki rendamen 45,86 dengan kadar total fenol dan flavonoid 0,34 dan 0,02 dan mengandung apigenin, kaemferol, kuersetin dan rutin dengan kadar kuersetin 5,75 . Fraksi aktif memiliki IC50 802,42 ppm dan LD50 > 5000 mg/kb bb sehingga aman digunakan. Semua dosis fraksi aktif dapat menurunkan konsentrasi tamoksifen dan 4-hidroksitamoksifen dalam plasma. Kromatografi Cair Kinerja Tinggi tandem Spektrometri Masa dapat mengukur konsentrasi tamoksifen dan 4-hidroksitamoksifen dalam plasma, penurunan itu diduga karena fraksi aktif yang diberikan menghambat proses metabolisme tamoksifen dengan demikian maka fraksi aktif berpotensi sebagai sebagai kemopreventif.

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ABSTRACT
Tamoxyfen is the first choice of drug treatment for breast cancer in women with estrogen receptor positive ER , however in the long term use of 5 10 years they are exposed to risk of secondary cancer in the form of endometrial cancer. A sensitive, specific and selective analysis method is required to measure the concentrations of tamoxyfen and 4 hydroksitamoxyfen in plasma as an attempt to predict the occurrence of secondary cancer and its effect after administration of active fraction against concentrations of tamoksifen and 4 hidroksitamoksifen using Liquid chromatography tandem mass spectrometry was developed in accordance with EMEA criteria. Myrmecodia erinacea Becc. was extracted in 80 ethanol by maceration to obtain 80 ethanol extracts and then fractination was perfomed with n heksan, ethyl acetate and butanol to obtain the active fraction afterward the chemical compounds were identified. Acute toxicity and cytotoxic test were performed against active fraction, then activity as chemoprevention of ant nest plant M. erinacea Becc. was performed on 30 female rats, divided into 6 treatments, which were given tamoxyfen 20 mg kb bb Positive control , aqua distillata Normal Control , and corn oil Negative Control . The test group was given a test fraction equivalent to 100, 200 and 400 mg kb bb doses of quercetin. Tamoxyfen 20 mg kg bw was administered in the whole group except negative control and normal control , then 30 minutes later the test fraction was given to the treatment group according to the dose, and was carried out for 20 days. Sensitive, specific and selective analysis method was developed on the calibration curve range 2.0 ndash 200.0 ng mL. The chosen active fraction was etilasetat with yield of 45.867 , which had the highest value of total phenol and its flavonoida of 0.34 and 0.02 thus containing apigenin, quercetin, kaemferol and rutine with levels of quercetin 5.75 . Active fraction containing IC50 was 802.84 ppm and LD50 5000 mg kg bw so it is safe to be used. All doses of the active fraction could lower concentrations of tamoxyfen and 4 hydroxytamoxifen in plasma. Liquid chromatography tandem Mass Spectrometry can measure concentrations of tamoxifen and 4 hydroxytamoxifen in plasma. The decline was allegedly because the active fraction inhibited metabolism of tamoxiifen, therefore active fraction had potential as as chemopreventive.