METHOD OPTIMIZATION AND VALIDATION OF DDIE, SAFROLE, AND MYRISTICIN ASSAY IN NUTMEG EXTRACT AND HERBAL TABLET BY GAS CHROMATOGRAPHY - MASS SPECTROMETER

• Main Author: Very E B A A, Bambang
• Format: Theses
• Language: Indonesia
• Online Access: https://digilib.itb.ac.id/gdl/view/78959
• Institution: Institut Teknologi Bandung

Nutmeg (Myristicafragrans Houtt.) is one of the spices origins from Indonesia that has been proven to be possessed an antidiabetic activity, as the active compound of dehydrodiisoeugenol (DDIE). Nutmeg also contains compounds that are poisonous and hallucinogenic, i.e. safrole and myristicin. The toxic compound elimination is being conducted by a process and formulated into tablets. Quality control should be conducted to quanti& DDIE, safrole, and myristicin. One of the instruments that can be used is gas chromatography conrfected to a mass spectrometer detector. The purpose of this study is Qdevelop the quantification method by optimizing Of instrument's system, conducting validation method, and applying on the samples. Optimization is conducting by capillary column Durabond@ DB-IMS (30.0 m x 0.25 mm x 0.25 um) and helium as carrier gas. The optimum instrument condition is obtained as follow. Initial temperature of column is regulated on 70 oc and holded for 5 minutes, elevated to 265 oc by ramp rate 30 OC/minute, and holded for 4.5 minutes. Helium flow is regulated at constant linear velocity on 40.2 cm/second. Sample injection is conducted by split method and injector temperature on 300 oc. Ion source temperature is set on 200 oc- Detection is being conducted by a selected ion monitoring (SIM) method on each molecule ion by event time at 0.10 seconds. This method has met validation requirements for system suitability test, selectivity/specificit% linearity, accuracy, repeatability precision, and robustness in normal condition. Detection limit of this method for DDIE, safrole, and myristicin is 9.68 gg/rnl, 0.04 ugh-nl, and 0.36 gg/ml, respectively, and quantification limit is 29.03 gg/ml, 0.12 ug/ml, and 1.09 ug/ml, respectively. Assay is being conducted on extract and tablet sample. DDIE, safrole, and myristicin content in nutmeg extract prior to process is 52.219 mg/g, 14.649 mg/g, and 172.053 mg/g, respectively; in nutmeg extract after the process is 29.688 mg/g, 0.044 mg/g, and 0.288 mg/g, respectively; and in tablet is 8.572 mg/tablet, 0.015 mg/tablet, and 0.094 mg/tablet, respectively. This method can be an alternative method for product quality control that fast, easy, sensitive, and selective.