Optimization of an Ultrasound-Assisted Extraction for Simultaneous Determination of Antioxidants in Sesame with Response Surface Methodology

• Main Authors: Dandan Wang (Author), Liangxiao Zhang (Author), Yueqing Xu (Author), Xin Qi (Author), Xuefang Wang (Author), Xiupin Wang (Author), Qi Zhang (Author), Peiwu Li (Author)
• Format: Book
• Published: MDPI AG, 2019-08-01T00:00:00Z.
• Subjects: article
• Online Access: Connect to this object online.
• Notes: 2076-3921; 10.3390/antiox8080321
• Keywords: antioxidants; ultrasound-assisted extraction; liquid chromatography-tandem mass spectrometry (LC-MS/MS); sesame; simultaneous detection; response surface methodology; Therapeutics. Pharmacology; RM1-950
• Source: Antioxidants, Vol 8, Iss 8, p 321 (2019)

Sesame is a nutritional agricultural product with medicinal properties. Accurate determination of micronutrients is important for the improvement of sesame quality and nutrition assessments. Our previous study showed that 10 antioxidants&#8212;<span style="font-variant: small-caps;">d</span>-homoproline, vitamin B₂, coniferyl aldehyde, hesperidin, phloretin, N-acetyl-<span style="font-variant: small-caps;">l</span>-leucine, <span style="font-variant: small-caps;">l</span>-hyoscyamine, ferulic acid, 5-methoxypsoralen, and 8-methoxypsoralen&#8212;in sesame were potential characteristic nutrients in sesame. Herein, simultaneous detection of 10 different types of antioxidants was developed by using ultrasound-assisted extraction coupled with liquid chromatography-tandem mass spectrometry (UAE-LC-MS/MS) with the help of response surface methodology. The significant variables and levels were screened and optimized by combining the single factor experiment, Plackett&#8722;Burman test, and Box&#8722;Behnken design. The optimal conditions for extraction of target antioxidants in sesame were methanol solution of 75.0%, liquid-to-material ratio of 20:1 (mL/g), extraction temperature of 50 &#176;C, extraction power of 410.0 W, extraction time of 65 min. The total yield of targets was 21.74 &#956;g/g under the optimized conditions. The mobile phase used was 0.1% formic acid in acetonitrile and 0.1% formic acid in water, and the column was a Thermo Syncronis C18 reverse phase column (100 mm &#215; 2.1 mm, 3 &#956;m). All targets required only one injection and could be quickly separated and assayed within 7 min. The limits of detection and limits of quantification for these 10 nutritional compounds ranged from 0.01 to 0.11 &#181;g/kg and from 0.04 to 0.34 &#181;g/kg, respectively. The validation results indicated that the method had reasonable linearity (<i>R</i>² &#8805; 0.9990), good recoveries (71.1%&#8722;118.3%), satisfactory intra-day precision (&#8804;9.6%) and inter-day precision (&#8804;12.9%), and negligible matrix effects (&#8804;13.8%). This simultaneous quantification method was accurate, fast, and robust for the assessment of sesame nutrition.