METHOD DEVELOPMENT FOR SIMULTANEOUS ANALYSIS OF STEROID AND NON STEROID ANTIINFLAMATORY SUBSTANCES IN JAMU PEGAL LINU USING TLC-SPECTROPHOTODENSITOMETRY

• Main Author: Aprilia Wisnuwardhani, Hilda
• Format: Theses
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/69901
• Institution: Institut Teknologi Bandung

Illegally added chemical adulteration of jamu become a problem that more difficult to stop. Therefore method development of simultaneous detection of chemical adulteration must be conducted. The aim of this research is to develop analytical method to detect simultaneously chemical adulteration in jamu pegal linu. Stationary phase, mobile phase, sample preparation and instrument condition were optimized. The result of optimization were validated for accuracy, precision (repeatability and intermediate precision), linearity, detection and quantitation limit. The validated methods were applied to analyze of eleven jamu pegal linu products in the market for the qualitative and quantitative analysis of chemical adulteration. Analytical method optimization showed that the best separation of five substances, acetaminophen, dexamethasone, prednisone, mefenamic acid and piroxicam was performed on silica gel GF254, using chloroform –methanol (9:1) as a mobile phase. Samples were prepared by extraction using ethanol as a solvent. Extraction was done for 30 minutes using 3D shaker. Chamber saturation was done for 60 minutes. Detection of chemical adulteration was performed using CAMAG TLC Scanner at ?254 nm for simultaneous detection, and at ?248 nm for quantitative analysis of acetaminophen. The calibration curve area versus concentration was found to be linear in the range of 200-1200 ng/ 5 µL. Linearity of analytical method gave a correlation factor, r = 0,9996 for TLC and r= 0,9982 for HPTLC. Linear regression coefficient of variance (Vx0) was calculated 1,66% for TLC and 3,57% for HPTLC. Detection and quantitation limit was calculated 34,907 ng and 116,356 ng for TLC; 74,991 ng and 249,972 ng for HPTLC. Recovery of analytical standard for three different concencentration was calculated 97,410 ± 0,83; 113,918 ± 9,931; 101,787 ± 2,769 for TLC, and 101,273 ± 0,826; 110,597 ± 8,867; 103,863 ± 3,417 for HPTLC. Intra day precision of the method was found 0,856%; 8,718%; 2,720% for TLC; and 0,816%; 7,836%; 3,290% for HPTLC. Inter day precision of the method was found 13,849%; 5,619%; 5,683% for TLC, and 6,269%; 2,945%; 4,735% for HPTLC. A new validated methods for qualitative analysis (acetaminophen, dexamethasone, prednisone, mefenamic acid and piroxicam) by thin layer chromatography (TLC) at ?254 nm and quantitative (acetaminophen) analysis of illegally added chemical adulteration of jamu pegal linu was developed by TLC-spectrophotodensitometry at ?248 nm. The separation was performed on silica gel GF254, using chloroform –methanol (9:1) as mobile phase. The methods can be used to analyze jamu pegal linu in the market.