OBJECTIVE: In this study, we report a rapid method for the residue analysis of IND and its metabolites, viz., IND-carboxylic acid, diaminotriazine, and triazine indanone in a wide range of palm oil matrices using liquid chromatography-tandem mass spectrometry (LC-MS/MS).
METHOD: The optimized sample preparation workflows included two options: (1) acetonitrile extraction (QuEChERS workflow), followed by freezing at -80°C and (2) acetonitrile extraction, followed by cleanup through a C18 solid phase extraction (SPE) cartridge. The optimized LC runtime was 7 min. All these analytes were estimated by LC-MS/MS multiple reaction monitoring.
RESULTS: Both sample preparation methods provided similar method performance and acceptable results. The limit of quantification (LOQ) of IND, IND-carboxylic acid, and triazine indanone was 0.001 mg/kg. For diaminotriazine, the LOQ was 0.005 mg/kg. The method accuracy and precision complied with the SANTE/12682/2019 guidelines of analytical quality control.
CONCLUSIONS: The potentiality of the method lies in a high throughput analysis of IND and its metabolites in a single chromatographic run with high selectivity and sensitivity. Considering its fit-for-purpose performance, the method can be implemented in regulatory testing of IND residues in a wide range of palm oil matrices that are consumed and traded worldwide.
HIGHLIGHTS: This work has provided a validated method for simultaneous residue analysis of indaziflam and its metabolites in crude palm oil and its derived matrices with high sensitivity, selectivity, and throughput.
OBJECTIVE: The purpose of this work was to transesterify the CCO in the presence of Candida antarctica lipase as catalyst and methanol. Additionally, the physicochemical parameters/fuel properties of the Citrullus colocynthis methyl ester (CCME) were assessed and compared.
METHODS: Lipase-catalyzed reactions were carried out in three necked flask (50 mL) attached with reflux condenser and thermometer, immersed in oil bath at constant stirring speed (400 rpm). The reaction mixture was consisted of CCO and varying the calculated amount of methanol, tert-butyl alcohol, and Novozym 435. The experimental parameters reaction time, methanol/oil molar ratio, reaction temperature, tert-butanol content, Novozym 435 content and water content were optimized for the transesterification reaction. The CCME yield was measured using gas chromatograph. The fuel properties of the produced CCME were determined as per American Society for Testing and Materials (ASTM) and European (EN) biodiesel standard methods.
RESULTS: In this study, an enzymatic catalyst was employed to synthesize the CCME from CCO via transesterification. Several variables affecting the CCME yield were optimized as lipase quantity (4%), water content (0.5%), methanol/oil molar ratio (5:1), reaction temperature (43 °C), reaction medium composition (80% tertbutanol/ oil), and reaction time (3.7 h). A CCME yield of 97.8% was achieved using enzyme catalyzed transesterification of CCO under optimal conditions. The significant biodiesel fuel properties of CCME, i.e. cloud point (0.70 °C); cetane number (49.07); kinematic viscosity (2.27 mm2/s); flash point (143 °C); sulfur content (2 ppm) density (880 kg/m3) and acid value (0.076 mg KOH/g) were appraised. CCME also exhibited long-term storage stability (4.80 h) and all the biodiesel fuel properties were within the range of standards (ASTM D6751 and EN 14214).
CONCLUSION: The lipase-catalyzed transesterification produced better conversion than the base-catalyzed reaction. The fuel properties of CCME were within the limits of the ASTM D6751 and EN14214 standards. Furthermore, CCME showed good oxidative stability and a long shelf life due its high natural antioxidant content. CCME showed better fuel properties and long-term storage stability due to which it can be used as a potential alternative fuel.