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. Sugiyanto
Lampung University
Biochemistry, Genetics & Molecular Biology Health Professions Mechanical Engineering Medicine & Pharmacology

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Validasi Metode Penetapan Kadar Lisinopril dalam Spiked Plasma Secara Ultra Performance Liquid Chromatography Melalui Derivatisasi dengan 1-Fluoro 2,4 Dinitrobenzen Sumiyani, Ririn; Martono, Sudibyo; Sugiyanto, .
JFIOnline | Print ISSN 1412-1107 | e-ISSN 2355-696X Vol 8, No 1 (2016)
Publisher : Indonesian Research Gateway

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Abstract

ABSTRACT: A rapid, accurate, and sensitive method for determining lisinopril in spiked plasma was developed by means using an Ultra Performance Liquid Chromatography (UPLC) with 1-fluoro 2,4 dinitrobenzen (FDNB) derivatization. Lisinopril was precolumn derivatized with FDNB at optimum condition, i.e. room temperature and borate buffer at pH 11, subsequently analyzed with UPLC. Isocratic condition of acetate buffer (0.01 M, pH 3.50) : acetonitrile : metanol = 70 : 10 : 20 (v/v/v) as mobile phase, 0.3 mL/min of flow rate at λ 296 nm were applied at Acquity BEH C18 column, resulting a linearity of lisinopril at range of concentration of 5,0-100 ng/mL (Y = 410,59x + 211,91, r = 0.93). The accuration of the established method was achieved by 88,59±6,01 to 101,70± 2,56% recovery, while the precision was shown with RSD value of 2,57- 8,16 %, limit of detection (LOD) instrument of 0,73 ng/mL and limit of quatification (LOQ) 2,44 ng/mL, dwith R2 = 0,9987 dan r = 0,9993. In addition, the resulted LOD and LOQ more or less similar with the published HPLC-MS-MS method (1.03-10.0 ng/mL). Hence, it could be concluded that the developed UPLC method can be used as an alternative method for determining lisinopril in plasma.Keywords: Lisinopril, FDNB, derivatization, UPLCABSTRAK: Penetapan kadar lisinopril dalam spiked plasma secara Ultra Performance Liquid Chromatography (UPLC) melalui derivatisasi dengan 1-fluoro 2,4 dinitrobenzen (FDNB) merupakan metode yang cepat, sensitif dan akurat. Derivatisasi precolumn lisinopril dan FDNB optimum pada suhu kamar, suasana dapar borat pH 11,0, dilanjutkan analisis secara UPLC isokratis menggunakan kolom Acquity BEH C dan fase gerak dapar asetat (0,01 M pH 3,50): asetonitril:metanol (70: 10: 20, v/v/v), laju alir 0,3 mL/menit pada λ 296 nm, menghasilkan linieritas kadar lisinopril dalam spiked plasma pada rentang 5,0 -100 ng/mL terhadap luas area lisinopril-DNB dengan persamaan Y = 410,59x + 211,91 dengan R2 = 0,9987 dan r = 0,9993 Akurasi metode ditunjukkan dengan nilai % rekoveri sebesar 88,59±6,01 smpai dengan 101,70± 2,56 %. Ketelitian ditunjukkan dengan nilai RSD 2,57- 8,16 %, sedangkan Batas Deteksi Instrumen = 0,73 ng/ mL dan Batas Kuantitasi = 2,44 ng/mL. Hasil Batas Deteksi penelitian ini relatif sama dengan Batas Deteksi penetapan kadar lisinopril secara HPLC-MS (1,03- 10,0 ng/mL). Dengan demikian dapat disimpulkan bahwa metode ini berpotensi dikembangkan sebagai metode alternatif pengganti HPLC-MS untuk penetapan lisinopril dalam plasma.Kata kunci: Lisinopril, FDNB, derivatisasi, UPLC
Validasi Metode Penetapan Kadar Lisinopril dalam Spiked Plasma Secara Ultra Performance Liquid Chromatography Melalui Derivatisasi dengan 1-Fluoro 2,4 Dinitrobenzen Sumiyani, Ririn; Martono, Sudibyo; Sugiyanto, .
Jurnal Farmasi Indonesia Vol 8, No 1 (2016)
Publisher : Jurnal Farmasi Indonesia

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (418.293 KB) | DOI: 10.35617/jfi.v8i1.417

Abstract

ABSTRACT: A rapid, accurate, and sensitive method for determining lisinopril in spiked plasma was developed by means using an Ultra Performance Liquid Chromatography (UPLC) with 1-fluoro 2,4 dinitrobenzen (FDNB) derivatization. Lisinopril was precolumn derivatized with FDNB at optimum condition, i.e. room temperature and borate buffer at pH 11, subsequently analyzed with UPLC. Isocratic condition of acetate buffer (0.01 M, pH 3.50) : acetonitrile : metanol = 70 : 10 : 20 (v/v/v) as mobile phase, 0.3 mL/min of flow rate at λ 296 nm were applied at Acquity BEH C18 column, resulting a linearity of lisinopril at range of concentration of 5,0-100 ng/mL (Y = 410,59x + 211,91, r = 0.93). The accuration of the established method was achieved by 88,59±6,01 to 101,70± 2,56% recovery, while the precision was shown with RSD value of 2,57- 8,16 %, limit of detection (LOD) instrument of 0,73 ng/mL and limit of quatification (LOQ) 2,44 ng/mL, dwith R2 = 0,9987 dan r = 0,9993. In addition, the resulted LOD and LOQ more or less similar with the published HPLC-MS-MS method (1.03-10.0 ng/mL). Hence, it could be concluded that the developed UPLC method can be used as an alternative method for determining lisinopril in plasma.Keywords: Lisinopril, FDNB, derivatization, UPLCABSTRAK: Penetapan kadar lisinopril dalam spiked plasma secara Ultra Performance Liquid Chromatography (UPLC) melalui derivatisasi dengan 1-fluoro 2,4 dinitrobenzen (FDNB) merupakan metode yang cepat, sensitif dan akurat. Derivatisasi precolumn lisinopril dan FDNB optimum pada suhu kamar, suasana dapar borat pH 11,0, dilanjutkan analisis secara UPLC isokratis menggunakan kolom Acquity BEH C dan fase gerak dapar asetat (0,01 M pH 3,50): asetonitril:metanol (70: 10: 20, v/v/v), laju alir 0,3 mL/menit pada λ 296 nm, menghasilkan linieritas kadar lisinopril dalam spiked plasma pada rentang 5,0 -100 ng/mL terhadap luas area lisinopril-DNB dengan persamaan Y = 410,59x + 211,91 dengan R2 = 0,9987 dan r = 0,9993 Akurasi metode ditunjukkan dengan nilai % rekoveri sebesar 88,59±6,01 smpai dengan 101,70± 2,56 %. Ketelitian ditunjukkan dengan nilai RSD 2,57- 8,16 %, sedangkan Batas Deteksi Instrumen = 0,73 ng/ mL dan Batas Kuantitasi = 2,44 ng/mL. Hasil Batas Deteksi penelitian ini relatif sama dengan Batas Deteksi penetapan kadar lisinopril secara HPLC-MS (1,03- 10,0 ng/mL). Dengan demikian dapat disimpulkan bahwa metode ini berpotensi dikembangkan sebagai metode alternatif pengganti HPLC-MS untuk penetapan lisinopril dalam plasma.Kata kunci: Lisinopril, FDNB, derivatisasi, UPLC
Co-Authors . Martinus, . . Tarkono, . . Zulhanif Ari Beni Santoso Dodi Marlin, Dodi Edy Meiyanto Efri Mahmuda, Efri Imam Munandar Imran Oktariawan, Imran M.Ikhsan Taufik, M.Ikhsan Nunuk Aries Nurulita Rahmat Iskandar Fajri, Rahmat Iskandar Ririn Sumiyani Shirley Savetlana, Shirley Sudibyo Martono Syamsul Arif Sarifudin, Syamsul Arif Teguh Sugiarto, Teguh