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Development and Validation GC/MS Method for Methamphetamine Analysis in Urine by Miniaturization QuEChERS Soraya Aulia; Riesta Primaharinastiti; Djoko Agus Purwanto
Science and Technology Indonesia Vol. 8 No. 3 (2023): July
Publisher : Research Center of Inorganic Materials and Coordination Complexes, FMIPA Universitas Sriwijaya

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.26554/sti.2023.8.3.451-460

Abstract

This paper explains the development of a quick and easy gas chromatography (GC) approach to identify methamphetamine in urine. This research used gas chromatography with mass spectroscopy and a capillary column TG-5SILMS (5% phenyl methyl siloxane, 30 m x 0.32 x 25 m). The carrier gas flow rate was set at 1.0 mL/minute, the temperature inlet and detector had been set at 300°C, and the oven temperature was programmed to initiate at 50°C and held for 1.5 minutes before being raised to 300°C at a rate 40°C/minute and held for 3 minutes. Sample pre-treatment by modification of the QuEChERS method includes using a relatively large amount of inorganic salt, extraction volume and extraction cycle. The optimal conditions for processing a 400 uL urine sample were 160 mg magnesium sulphate, 40 mg sodium chloride, and 400 uL acetonitrile for organic solvent. According to the validation test, the detection limit for methamphetamine was 0.36 ug/mL; the quantitation limit was 1.09 ug/mL, and the calibration curve followed the regression line. y=1.0489x-3.7914, coefficient (r) was 0.9973. The recovery of the analyte spiked into urine at 5, 7 and 9 ug/mL on average was 100.5±2.33% for intraday dan 93.3±7.21% for interday. The precision was excellent, with an average coefficient of variation of 2.31%. The procedure was applied to four urine samples from drug users and the first abuser (25.51 ug/mL), the second abuser (15.05 ug/mL), the third abuser (17.72 ug/mL) and the last abuser (3.08 ug/mL) were all satisfactorily quantitated.
Optimization and Prevalidation of TLC-Densitometry Method for Fucoidan Analysis in Sargassum sp. Aqueous Extract Laili Irfanah; Mochammad Yuwono; Riesta Primaharinastiti
JURNAL FARMASI DAN ILMU KEFARMASIAN INDONESIA Vol. 10 No. 2 (2023): JURNAL FARMASI DAN ILMU KEFARMASIAN INDONESIA
Publisher : Universitas Airlangga

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.20473/jfiki.v10i22023.210-216

Abstract

Background: Fucoidan is sulfated polysaccharide that has gastroprotector activity, and it is distributed in brown algae cell walls. Currently, there is no method for fucoidan analysis in compendia. Furthermore, analysis of Fucoidan is proven to be challenging due to the lack of chromophores and its high polarity. Objective: To develop the optimal condition of TLC-Densitometry method for fucoidan analysis in Sargassum sp. aqueous extract and to evaluate the stability of Fucoidan as a preliminary study. Methods: Chromatography was performed on Silica gel 60F254 TLC-plate as a stationary phase. The developed plate was stained with H2SO4 10% in absolute ethanol and heated in oven at 105°C for 15 minutes. Optimization is carried out by determining composition of the mobile phase, analytical wavelength, and spotting volume. Stability test of Fucoidan in standard and extract solution at 0, 4, 8, and 24 hours also 0 and 60 minutes after derivatization. Results: The optimal condition which produces a good separation of Fucoidan was achieved by using n-butanol:methanol: water (10:6:10 v/v/v) as a mobile phase, 400 nm as an analytical wavelength, and 1 µl as a spotting volume. Fucoidan was stable after storage until 24 hours. The stained spots were stable until 60 minutes after derivatization. Conclusion: Optimal condition of the TLC-Densitometry method for Fucoidan analysis was selective and can be applied to stability tests in preliminary study. Fucoidan was stable in standard solution and extracted solution until 24 hours after storage at 4°C, and the stained spots were stable until 60 minutes after derivatization.
Comparative Study of Densitometry and Videodensitometry for Quantitating the Active Pharmaceutical Ingredients Using Thin Layer Chromatography – Systematic Review Firmansyah Ardian Ramadhani; Idha Kusumawati; Riesta Primaharinastiti; Subhan Rullyansyah; Fajar Jamaluddin Sandhori; Hanif Rifqi Prasetyawan
JURNAL FARMASI DAN ILMU KEFARMASIAN INDONESIA Vol. 10 No. 2 (2023): JURNAL FARMASI DAN ILMU KEFARMASIAN INDONESIA
Publisher : Universitas Airlangga

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.20473/jfiki.v10i22023.141-150

Abstract

Background: Chromatography is one of the analytical techniques widely used for the quality control process in the pharmaceutical industry. One of the analytical methods used in drug analysis is Thin Layer Chromatography (TLC). The analysis process of TLC can be performed using densitometry (scanner) or videodensitometry (videoscan). The principal analysis of densitometry (scanner) is based on the density measured from each spot on the TLC plate using a specific wavelength range, and videodensitometry (videoscan) is performed by taking pictures of the plate using a Visualizer at a specific wavelength. Objective: This review article discusses the application of densitometry and videodensitometry methods for quantitative analysis of pharmaceutical products. Methods: This study was conducted using a systematic review method using the PRISMA statement from January to April 2023. Four databases were searched: PubMed, ScienceDirect, Scopus, and Google Scholar with inclusion criteria: studies on thin layer chromatography analysis using densitometry and videodensitometry. Results: Based on the ten articles in this study, it is known that the active ingredient concentrations in pharmaceutical products can be determined using densitometry and videodensitometry. The statistical analysis results show no significant difference between the two methods' chemical concentrations of active ingredients in pharmaceutical products. Conclusion: TLC densitometry and videodensitometry is a valid methods analysis that can be used for quantitating the active pharmaceutical ingredient concentration in finished pharmaceutical products.
AKTIVITAS AGEN TROMBOLITIK DAUN PEGAGAN (Centella asiatica) HASIL FERMENTASI OLEH Acetobacter aceti FNCC 0016 DENGAN METODE CLOT LYSIS SECARA IN-VITRO Adristy Ratna Kusumo; Achmad Toto Poernomo; Riesta Primaharinastiti
Jurnal Ilmiah Manuntung: Sains Farmasi Dan Kesehatan Vol. 7 No. 2 (2021): Jurnal Ilmiah Manuntung: Sains Farmasi Dan Kesehatan
Publisher : Sekolah Tinggi Ilmu Kesehatan Samarinda

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.51352/jim.v7i2.499

Abstract

Thrombolytic agents are plasminogen activators which can dissolve blood clot that caused cardiovascular disease (CVD). Thrombolytic agents can be obtained from microorganism such as Acetobacter aceti FNCC 0016 and from plants such as Centella asiatica, these thrombolytic agents are combined using fermentation method. Fermentation can improves the pharmacological properties of plants through modification of their metabolites. Fermentation mediated by microorganism has been shown to enhance the therapeutic efficacies of some plants. This research aimed to determine the increase of thrombolytic activity from the fermentation product of Centella asiatica by Acetobacter aceti FNCC 0016. Fermentation was carried out at various times (0 h, 24 h, 48 h, 72 h) at a temperature of 30±1°C. The thrombolytic activity was determined using in-vitro clot lysis method. The results showed a significant increase in thrombolytic activity after 72 hours of fermentation with thrombolytic index of 91,49 compared to Centella asiatica extract (42.93) and Acetobacter aceti FNCC 0016 (19.99). Conclusion: Thus, Centella asiatica that has undergone a fermentation process with Acetobacter aceti FNCC 0016 can increase the thrombolytic activity.