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Validasi Metode Analisis Bahan Pembanding Sekunder Anhidrotetrasiklin Hasil Transformasi In Situ Tetrasiklin Hidroklorida dengan Asam Hidroklorida Fajar Kurniyati; Asep Saefumillah
Sainsmat : Jurnal Ilmiah Ilmu Pengetahuan Alam Vol 3, No 1 (2014): Maret
Publisher : Fakultas Matematika dan Ilmu Pengetahuan Alam Universitas Negeri Makassar

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.35580/sainsmat3110142014

Abstract

Parameter mutu dan keamanan obat seringkali dikaitkan dengan kandungan cemaran di dalamnya terutama terkait dengan cemaran yang bersifat racun atau karsinogenik. Dalam konteks pengawasan obat di Indonesia, analisis yang akurat dalam mendeteksi dan mengkuantisasi cemaran pada senyawa obat maupun produk obat perlu dilakukan. Namun demikian, ketersedian bahan pembanding cemaran yang merupakan salah satu faktor penentu jaminan mutu hasil pengujian laboratorium, seringkali menjadi kendala karena sukar diperoleh dan cukup mahal harganya. Penelitian ini dimaksudkan untuk membuat bahan pembanding sekunder cemaran secara in situ dengan cara mengubah senyawa aktifnya dalam hal ini anhidrotetrasiklin hidroklorida yang dibuat melalui transformasi tetrasiklin hidroklorida dengan asam hidroklorida. Analisis kualitatif pada penelitian ini dilakukan dengan menggunakan HPLC yang dilengkapi detektor dioda array, sementara analisis kuantitatifnya dilakukan menggunakan HPLC UV-vis pada panjang gelombang 280 nm. Anhidrotetrasiklin hasil transformasi diuji stabilitasnya dengan microwave dan paparan sinar matahari dan hasilnya menunjukkan bahwa senyawa yang terbentuk bukan produk intermediet. Semua parameter validasi metode seperti spesifisitas/selektivitas, rentang, linearitas, presisi dan akurasinya telah terpenuhi dengan nilai sangat baik. Uji homogenitas juga dilakukan dan tetrasiklin hidroklorida yang diuji dapat dinyatakan homogen dalam hal pembentukan anhidrotetrasiklin hidroklorida. Nilai yang ditetapkan terhadap baku pembanding primer anhydrotetracycline hydrochloride EPRS adalah 102,05%, n=10, SD=0,64%, RSD=0,63% tanpa data outlier. Nilai estimasi ketidakpastian pengukuran diperluas yaitu 3,19%.Kata kunci: bahan pembanding sekunder in situ, anhidrotetrasiklin hidroklorida, transformasi, tetrasiklin hidroklorida, validasi metode, homogenitas
Development Study of Binding Agent in Diffusive Gradient In Thin Films (DGT) Technique for Absorption of Phosphate Compounds using Nano-La2O3 Hanna Shafira; Rika Tri Yunarti; Asep Saefumillah
Jurnal Kimia Valensi Jurnal Kimia VALENSI Volume 8, No. 2, November 2022
Publisher : Syarif Hidayatullah State Islamic University

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.15408/jkv.v8i2.26952

Abstract

The abundance of phosphate is a concern because it causes problems in aquatic ecosystems. The diffusive gradient in thin films (DGT) technique is a promising method for phosphate absorption because it can be used in situ. The DGT device consists of a membrane filter, a diffusive gel, and a binding gel. The presence of a binding agent in the binding gel makes the specific analyte bound to the binding gel. One of the binding agents that can be used for phosphate absorption is La2O3. Binding gel La2O3 was successfully synthesized that proven by the similarity of FTIR peaks of the diffusive gel and binding gel. The typical absorption of La-O also proves it from the binding gel at 642 cm-1 and 423 cm-1. La2O3 binding gel was made of N,-N'-methylenebisacrylamide as a cross-linker with an elution factor of 97.4%. DGT-La2O3 proved capable of adsorption for 72 hours, with phosphate absorbed at 1.91 x 105 ng. DGT-La2O3 also has the optimum ability to absorb phosphate at pH 3 of 1.93 x 105 ng.
Studi Bioavailabilitas Logam Berat Merkuri Secara Ekstraksi Bertahap Dan Difussive Gradient In Thin Films (DGT) Pada Tanaman Bayam Batik (Amaranthus Tricolor L) Helmiady Helmiady; Asep Saefumillah; Budiawan Budiawan
Syntax Literate Jurnal Ilmiah Indonesia
Publisher : Syntax Corporation

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (802.001 KB) | DOI: 10.36418/syntax-literate.v7i11.9902

Abstract

Tanah adalah sumber alami yang penting dan merupakan bagian dari lingkungan. Merkurimerupakan salah satu logam yang memiliki dampak toksisitas yang berbahaya bagi manusia. Metode untuk ekstraksi bertahap untuk merkuri pada tanah. Merkuri dipisahkan menjadi fraksi- fraksi. Urutan lima langkah ekstraksi F1 (air deionisasi), F2 (0,01 M HCl + 0,1 M CH3COOH), F3(1 M KOH), F4 (12 M HNO3), dan F5 (aqua regia). Dari antara fraksi tersebut yang terbesar adalah: merkuri terikat sulfida (57,08 - 94,53%) dan merkuri unsur (4,79 - 6,10 %). Fraksi terkecil adalah merkuri larut asam (0,21 – 0,73%), merkuri larut air (0,45 – 0,68 %) dan senyawa organomerkuri (0,33 – 0,68%). Teknik Diffusive Gradients in Thin Films (DGT) merupakan metode yang dikembangkan untuk monitoring partikel logam berat pada media baik perairan, sedimen dan tanah. Namun, dilakukan modifikasi pada salah satu komponen difussive gelnya, yaitu Crosslinker (pengikat silang) dengan menggunakan N,N’-methylenebisacrylamide (MBA) yang dikombinasikan dengan agarosa sebagai difusif gel, serta penggunaan resin gel 3- mercaptopropyl-terfungsionalisasi silika gel (komersil). Nilai koefisien elusi adalah 0,73, sedangkan nilai koefisien difusi 1,025 x 10-6 cm2/s. Keseluruhan analisis menggunakan teknik Cold Vapor-Atomic Absorption Spectrometry. Nilai CDGT-Hg berkisar 8, 6074 – 19,8790 µg/L, sedangkan C A.tricolor 0,087 – 2,074 µg/kg.
Metabolite Formation of Pesticide Isoprocarb in Coffee Beans During Short-Term Storage and Condition Rosaria Nainggolan; Asep Saefumillah; Endang Saefudin; Yanwar Pratama Putra
Jurnal Kimia Sains dan Aplikasi Vol 27, No 2 (2024): Volume 27 Issue 2 Year 2024
Publisher : Chemistry Department, Faculty of Sciences and Mathematics, Diponegoro University

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.14710/jksa.27.2.45-52

Abstract

Isoprocarb (IPC) is one of the most important carbamate pesticides for white flea control in coffee plants. The prevalence of isoprocarb pesticide residues in coffee, i.e., green coffee beans, is a cause for concern. Green coffee beans were intentionally contaminated with isoprocarb at concentrations >0.01 mg/kg, which was investigated in this research. Quantitative analysis of isoprocarb with the QuEChERS method and qualitative analysis for metabolite formation was characterized using UV-Vis, FTIR, 1H-NMR, GC-MS, and LC-QTOF-MS. Based on the data, the metabolite formed is o-cumenol through the hydrolysis reaction of o-aryl carbamate with the enzyme carboxylesterase. o-cumenol or 2- isopropylphenol as a phenol derivative. To verify the existence of metabolite analytes that are believed to be there in coffee tainted with isoprocarb, more reliable analytical techniques utilizing analytical standards must be developed. Isoprocarb concentrations decreased along the storage time, especially in unsterilized conditions. As a toxic compound, a quantitative structural activity relationship study (QSAR) was initially carried out through a software application for estimating toxicity (TEST) provided by the US Environmental Protection Agency (EPA). For additional information, based on the LC50 and LD50 data confirmed from the TEST application, it was concluded that isoprocarb is more toxic than o-cumenol.
Adsorption Study of Methylene Blue and Methyl Red on Activated Carbon from Silver Composite Using the Extract of Spent Coffee Grounds Haidar Sitie Rafidah; Hafiizh Prasetia; Asep Saefumillah
Jurnal Sains Materi Indonesia Vol. 25 No. 2 (2024): Jurnal Sains dan Materi Indonesia
Publisher : BRIN Publishing (Penerbit BRIN)

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.55981/jsmi.2024.924

Abstract

The activated carbon was prepared from silver composite via an extract of spent coffee grounds with phosphoric acid activation. The activated carbon was used to study the removal of methylene blue and methyl red from an aqueous medium. Fourier-transform infrared spectroscopy (FTIR) spectra confirmed the functional group of O–P–O that can interact with dye molecules and the reduction process of Ag+ to Ag0. Field Emission Scanning Electron Microscopy (FESEM) morphology suggests a porous and irregular polygonal shape. The efficiency removal and adsorption capacity of methylene blue reached 98.73% and 9.87 mg/g at pH 9, while methyl red reached 98.55% and 9.86 mg/g at pH 4. The kinetics adsorption study followed the pseudo-first order. The isotherm adsorption study followed the Langmuir model. Based on the kinetics and isotherm study, the adsorption study of methylene blue and methyl red is chemical sorption.
Advanced electrochemical detection of arsenic using platinum-modified boron-doped diamond by anodic stripping voltammetry Fatah, Fadhlir R. A. A.; Sitorus, Rinaldo; Saefumillah, Asep; Mubarok, Hanif; Pramadewandaru, Respati K.
Environmental and Materials Vol. 2 No. 1: (June) 2024
Publisher : Institute for Advanced Science, Social, and Sustainable Future

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.61511/eam.v2i1.2024.993

Abstract

Background: Platinum-modified boron-doped diamond (BDD) electrodes were effectively fabricated through a combination of wet seeding and electrodeposition techniques. Methods: This research involved the utilization of various chemicals and apparatus, the modification of boron-doped diamond (BDD) electrodes with platinum using wet seeding and electrodeposition, and the detection of As3+ and As5+ using a phosphate buffer solution and anodic stripping voltammetry (ASV). Findings: Characterization using Scanning Electron Microscopy-Energy Dispersive Spectroscopy (SEM-EDS) confirmed the successful deposition of 1.54% platinum on the BDD surface. These modified electrodes were employed as sensors for arsenic species (As³⁺ and As⁵⁺) using anodic stripping voltammetry (ASV) in a 0.1 M phosphate buffer solution at pH 6. Under optimal conditions, including a deposition potential of -500 mV, a deposition time of 150 s, and a scan rate of 200 mV/s, the linear detection of As³⁺ and As⁵⁺ was achieved within a concentration range of 0 to 100 ppb (R² = 0.9797 and 0.9903, respectively). Prior to ASV detection of As⁵⁺, a pretreatment step involving the addition of 0.1 M NaBH₄ was necessary to reduce As⁵⁺ to As³⁺. The detection limits for As³⁺ and As⁵⁺ were determined to be 16.50 ppb and 8.19 ppb, respectively. Conclusion: This research highlights the potential of BDD/Pt electrodes in environmental monitoring and arsenic detection applications and demonstrates the method's efficacy for the speciation analysis of arsenic species. Novelty/Originality of this Study: This research pioneers the use of platinum-modified boron-doped diamond electrodes for the speciation analysis of arsenic, offering a promising new approach for environmental monitoring applications.
Zeolite from Zirconium-Modified Fly Ash Waste for Absorption of Phosphate Compounds in Waters Putri, Mu'izzah Irsyadi; Saefumillah, Asep; Bakri, Ridla
Jurnal Kimia Valensi Jurnal Kimia VALENSI Volume 9, No. 1, May 2023
Publisher : Syarif Hidayatullah State Islamic University

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.15408/jkv.v9i1.26951

Abstract

Eutrophication is a phenomenon of decreasing air quality caused by the very high amount of phosphate ions in the aquatic system. Thus, an effective and efficient adsorbent is needed for phosphate absorption in aquatic systems. In this study, zeolit from fly ash waste was modified with zirconium (Zr) as an adsorbent for phosphate absorption in aquatic systems. Fly ash was pretreated with acid and then synthesised using the hydrothermal method. And then, the results of the fly ash zeolit synthesis were continued using zirconium. The adsorption capacity was tested through several parameters, including the adsorbent concentration test, variations in pH,and contact time. Zirconium-modified zeolite (ZrMZ) adsorbent was the most effective adsorbent for phosphate adsorption, with an adsorption capacity of 3.015 mg-P/g at a 3 g/L adsorbent dosage and pH 7. The adsorption kinetics for the ZrMZ adsorbent followed pseudo-second-order kinetics. The best result of ZrMZ adsorbent to absorb phosphate in lake water was an adsorption capacity value of 0.186 mg-P/g and an adsorption efficiency of 81.137%.
Characterization Study of Dyes Photodegradation-Adsorption Products by TiO2-Chitosan Immobilized on Glass Beads using Flow System Mahadika, Bella Sukma; Saefumillah, Asep; Saepurahman, Saepurahman; Kurnia, Kiki Adi; Wellia, Diana Vanda
Jurnal Kimia Valensi Jurnal Kimia VALENSI Volume 9, No. 1, May 2023
Publisher : Syarif Hidayatullah State Islamic University

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.15408/jkv.v9i1.31855

Abstract

Dyes have a complex molecular structure that is difficult to degrade and can persist for a long time in water bodies. This study examines more thoroughly the effectiveness of photodegradation-adsorption of dyes, kinetic aspects, isotherms, thermodynamics, identification of the structure of photodegradation products, and changes in environmental quality parameter values whose results are quite satisfactory. The combination of photodegradation-adsorption of dyes by TiO2-chitosan modified glass beads using a flow system has never been accomplished before. Flowing of the dye resulted in a dye degradation efficiency of 99%. The FESEM-EDX analysis shows that TiO2-chitosan has been coated onto the surface of the glass beads. R2 of kinetics MB, MO, RB are 0.99234, 0.9889, 0.9971, which were pseudo-first order. Qm, KL, R2 are 6.4382, 0.70533, 0.99923; 16.7364, 1.42059, 0.98816; 6.0078, 1.06973, 0.99889, respectively. The ∆H, ∆S, ∆S of -9.388, -0.024, -1.979; -27.182, -0.078, -3.592; -4.819, -0.017, 0.464 indicate the exothermic and spontaneous reaction. COD, TOC, pH, turbidity values have reached the threshold required by the government. The degradation products formed during the photodegradation-adsorption process were identified using LC-MS that the structure of the dye has been degraded to become simpler so that it is safely disposed of into the environment.
Development and Validation of a Method for Detecting and Quantifying Mitragynine in Kratom Samples Using HPLC-PDA Isnaeni, Neni; Saefumillah, Asep; Cahyana , Antonius Herry
Eruditio : Indonesia Journal of Food and Drug Safety Vol 4 No 2 (2024): June Edition
Publisher : Badan Pengawas Obat dan Makanan

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.54384/eruditio.v4i2.209

Abstract

Kratom (Mitragyna speciosa Korth) has been identified as a New Psychoactive Substance (NPS) by the United Nations Office on Drugs and Crime (UNODC) and included in the list of prohibited ingredients in food supplements and traditional medicine by Indonesian FDA. Therefore, a rapid, easy, and reliable analytical method is necessary to detect and quantify this plant and its products. This study developed a method for the detection and quantification of kratom products based on a unique compound, mitragynine, as a biomarker. A previous survey of determining mitragynine in Kratom using GC-MS, LC-MS/MS, UPLC, and HPLC-PDA. Previously, the HPLC-PDA method used a C8 column. Yet, for efficiency, it is also necessary to develop a test method using a C18 column. Analysis was performed using an HPLC - PDA system with Waters Atlantis T3-C18 (250 x 4.6 mm, 5 µm) column. The mobile phase comprises acetonitrile and formic acid 0.05%, pH 5.0 (75:25 v/v), delivered at a 1.0 mL/min flow rate. Detection was carried out at a wavelength of 225 nm. The analytical method was validated with test parameters of selectivity, system suitability, accuracy, precision, linearity, detection limit, and quantification limit. The validation study demonstrated an excellent linear concentration range of 1.96 - 6.01 µg/mL with a correlation coefficient of 0.9996; the detection limit is 0.14 µg/mL, while the limit of quantification is 0.45 µg/mL—accuracy method of 98.88 - 101.44% and a bias of 0.27%. The percent relative standard deviation for six independent assay determinations was 0.67%, and the intermediate precision was 1.56% on two days. The mitragynine amounts in these materials ranged from 6.01 to 6.31 mg/g of dried leaf material. Based on the research results, it can be concluded that the method developed provides quick, simple, reliable, accurate, and valid, and has an advantage over existing methods in terms of simplicity of sample preparation, short analysis time, and cost-effectiveness compared to GCMS and LCMS/MS and can be applied for future analysis in Kratom samples.
Study on the Phosphate Compound Adsorption onto MgO-KOH/Biochar Adsorbent as Binding Agent in Diffusive Gradient in Thin Film (DGT) Technique for Bioavailable Phosphate Detection Permatasari, Indah; Saefumillah, Asep
Bulletin of Chemical Reaction Engineering & Catalysis 2024: BCREC Volume 19 Issue 3 Year 2024 (October 2024)
Publisher : Masyarakat Katalis Indonesia - Indonesian Catalyst Society (MKICS)

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.9767/bcrec.20178

Abstract

Phosphate compounds, particularly bioavailable forms like PO₄³⁻, are critical contributors to eutrophication. In this study, MgO-KOH/biochar was used as a binding agent in the Diffusive Gradient in Thin Films (DGT) technique to enhance phosphate detection. The adsorbent was synthesized from biochar derived from palm oil waste, activated with KOH to increase surface area, and combined with MgO for enhanced adsorption efficiency. The adsorption process followed a pseudo-second-order kinetic model, indicating that chemical interactions dominated the adsorption mechanism. Under different pH levels and phosphate concentrations, the material showed a good selectivity for orthophosphate, achieving an adsorption capacity of approximately 100 mg/g. Characterization via FTIR, XRD, and SAA confirmed the successful synthesis of MgO-KOH/biochar and its structural properties, which contributed to its performance. Additionally, the MgO-KOH/biochar DGT device demonstrated better efficiency in adsorbing PO₄³⁻ compared to conventional ferrihydrite-based DGT systems, positioning it as a highly effective tool for monitoring bioavailable phosphates in aquatic environments. Copyright © 2024 by Authors, Published by BCREC Publishing Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0).