scholarly journals ANALYTICAL METHOD OPTIMIZATION AND VALIDATION OF GLIBENCLAMIDE AND METFORMIN HYDROCHLORIDE IN DIABETIC HERBS PRODUCT BY THIN-LAYER CHROMATOGRAPHY-DENSITOMETRY

Author(s):  
BAITHA PALANGGATAN MAGGADANI ◽  
NOVIANI SUGIANTO ◽  
HAYUN

Objective: This study aimed to develop and validate an analytical method using thin-layer chromatography (TLC)-densitometry for detecting thepresence of glibenclamide and metformin hydrochloride in herbal diabetic products.Methods: The jamu samples were extracted using methanol, followed by analysis using TLC-densitometry with methanol-aquades-glacial acetic acid(9:1:0.25) as the mobile phase at a wavelength of 237 nm.Results: From the validation results, the correlation coefficients for glibenclamide and metformin hydrochloride were determined to be 0.9998and 0.9981, respectively. The limits of detection and quantitation for glibenclamide were 49.97 μg/mL and 66.55 μg/mL, respectively, while thoseof metformin hydrochloride were 74.75 μg/mL and 249.25 μg/mL, respectively. The method developed in this study met the criteria of selectivity,accuracy, and precision. From seven jamu samples tested, four tested positive for glibenclamide, with sample 1=4.9522%, sample 2=4.1495%, sample3=4.2578%, and sample 4=4.9412%.Conclusion: None of the jamu samples contained metformin hydrochloride.

2018 ◽  
Vol 10 (1) ◽  
pp. 51
Author(s):  
Viona Prima Dyta ◽  
Harmita . ◽  
Baitha Palanggatan M

Objective: The objective of this study was to obtain an optimum and valid method of analysis to determine the levels of disodium 5’-guanylate (DSG)and disodium 5’-inosinate (DSI) in six samples of spices.Methods: The optimum method was obtained using silica gel 60 F254 as the stationary phase and isopropanol:water:25% ammonia at a ratio of 6:3:1(v/v) as the mobile phase. The developed spots were scanned using a densitometer in absorbance mode at 260 nm. The methods were valid basedon the accuracy criteria (DSG, 99.11–99.96%, and DSI, 98.56–101.05%), precision (DSG, 1.09%, and DSI, 0.49%), and linearity (DSG, r=0.9909, andDSI, r=0.9976).Results: The results showed that the levels of DSG in samples A, B, C, D, E, and F were 0.70%, 0.79%, 0.78%, 0.99%, 1.08%, and 1.08% and those ofDSI were 0.66%, 0.74%, 0.71%, 0.66%, 0.54%, and 0.67%, respectively.Conclusion: The optimum conditions of DSG and DSI for thin-layer chromatography-densitometry were obtained with silica gel 60 F254 as thestationary phase, isopropanol:water:25% ammonia (6:3:1) as the mobile phase, and a maximum wavelength of about 260 nm. Validation resultsindicated that the accuracy of the analytical method for DSG was about 99.11–99.96% with a coefficient variation (precision) of 0.70–1.41%, whilethat for DSI was 98.56–101.05% with a coefficient variation of 0.23–0.75%. The correlation coefficients for the analytical method for DSG and DSIwere 0.9909 and 0.9976, respectively. The results determined that the levels of DSG and DSI in samples A, B, C, D, E, and F were 0.70%/0.60%,0.79%/0.74%, 0.78%/0.71%, 0.99%/0.66%; 1.08%/0.54%, and 1.08%/0.67%, respectively.


2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.


Talanta ◽  
1992 ◽  
Vol 39 (8) ◽  
pp. 953-958 ◽  
Author(s):  
I POLITZER ◽  
K CRAGO ◽  
K AMOS ◽  
K MITCHELL ◽  
T HOLLIN

2018 ◽  
Vol 1 (1) ◽  
pp. 264-270
Author(s):  
Hady Wiraputra ◽  
Marline Nainggolan ◽  
Panal Sitorus

Tanaman buni (Antidesma bunius (L.) Spreng.) secara tradisional telah digunakan untuk hipertensi, takikardia, anemia, sifilis, antikanker, antioksidan, sumber pewarna alami dan antidiabetes. Saponin merupakan senyawa fitokimia yang mempunyai kemampuan membentuk busa dan mengandung aglikon polisiklik yang berikatan dengan satu atau lebih gula. Penelitian ini bertujuan untuk melakukan karakterisasi senyawa saponin hasil isolasi dari daun buni dengan spektrofotometer ultraviolet dan inframerah. Simplisia daun buni dilakukan karakterisasi kemudian diekstraksi dengan cara maserasi bertingkat menggunakan pelarut n-heksana dan etanol 80%. Selanjutnya ekstrak etanol dihidrolisis dengan HCl 2N kemudian difraksi dengan pelarut kloroform. Isolasi dilakukan terhadap fraksi kloroform dengan cara kromatografi lapis tipis preparatif menggunakan fase diam silika gel GF254 dan fase gerak yang sesuai. Isolat yang diperoleh diuji kemurnian dengan KLT 2 arah dan dikarakterisasi menggunakan spektrofotometer ultraviolet dan inframerah. Hasil pemeriksaan karakterisasi simplisia diperoleh kadar air 7,32%, kadar sari larut dalam etanol 52,70%, kadar sari larut dalam air 23,25%, kadar abu total 6,86% dan kadar abu tidak larut dalam asam 0,94%. Pemisahan fraksi kloroform dengan KLT menggunakan fase gerak n-heksana-etilasetat perbandingan 5:5 diperoleh noda 13 dan hasil KLT preparatif diperoleh 2 isolat murni yaitu isolat 1 (ungu merah) dengan Rf 0,92 dan isolat 2 (biru) dengan Rf 0,78. Hasil karakterisasi isolat 1 diperoleh panjang gelombang maksimum pada 208 nm dan dijumpai adanya gugus hidroksil, gugus -CH alifatis, ikatan C=C, gugus –CH2, gugus –CH3, dan gugus C-O. Hasil karakterisasi isolat 2 diperoleh panjang gelombang maksimum pada 204 nm dan adanya gugus hidroksil, gugus -CH alifatis, gugus –CH2, gugus –CH3, dan gugus C-O. Buni (Antidesmabunius (L.) Spreng.) has been traditionally used for the treatment of hypertension, tachycardia, anemia, syphilis, and used asanti-cancer, anti-oxidant, natural dye, and anti-diabetic. Saponin is a phytochemical compound which has capability in forming foam and contains polycyclic aglycone that binds with one or more glucose. This research aimed to conduct the characterization of saponin compound from buni leaves with ultraviolet spectrophotometer and infrared. Buni leaves simplicia was characterizedand extracted using sequential maceration method with n-hexane and 80% ethanol. The ethanol extract was hydrolyzed with HCl 2N and fractionized using chloroform solvent. Isolation of chloroform fraction was done using preparative thin-layer chromatography using silent phase of silica gel GF 254 and suitable mobile phase. Isolates obtained was taken into purity test with two dimensions thin-layer chromatography and characterized using ultraviolet spectrophotometer and infrared. The characterized simplicia resulted with 7.32% of water content, 52.70% of dissolved content in ethanol, 23.25% of dissolvedcontent in water, 6.86% of total ash content, and 0.94% of undissolved ash content in acid. Fractinationof chloroform fraction with thin-layer chromatography using mobile phase ofn-hexane-ethyl acetate with 5:5 ration resulted with 13 spotsand the result of the preparative thin-layer chromatography resulted 2 pure isolates which are isolate 1 (purple-red) with Rf 0.92 and isolate 2 (blue) with Rf 0.78. The characterization of isolate 1 resulted that the maximum wave lengthwas 208 nm with hydroxyl group, –CH aliphatic group, C=C bond, –CH2 group, –CH3 group, and C–O group. The characterization of isolate 2 resulted that the maximum wave lengthwas204 nm with hydroxyl group, –CH aliphatic group, –CH2 group, –CH3 group, and C–O group.


1994 ◽  
Vol 77 (5) ◽  
pp. 1179-1183 ◽  
Author(s):  
Yichun Xu ◽  
C J Mirocha ◽  
W Xie

Abstract An analytical method was developed for the detection of fusarochromanone (TDP-1) in com and wheat by liquid chromatography. Extraction was done with methanol-water-ammonium hydroxide (90 + 10 + 2), and cleanup was by elution through a silica Sep-Pak cartridge. The limit of sensitivity of TDP-1, detected on the basis of its fluorescence properties, is 200 pg, whereas the detection limit of the method for corn and wheat is 5 ng/g. The average recoveries of TDP-1 added at 5,25,100,500, and 1000 ppb were 86% for corn and 83% for wheat. Confirmation was done by thin-layer chromatography.


Sign in / Sign up

Export Citation Format

Share Document