scholarly journals Extraction and Determination of Vitamin K1 in Foods by Ultrasound-Assisted Extraction, SPE, and LC-MS/MS

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 839 ◽  
Author(s):  
Yueqing Xu ◽  
Liangxiao Zhang ◽  
Ruinan Yang ◽  
Xu Yu ◽  
Li Yu ◽  
...  
Keyword(s):  
Formic Acid ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Extraction Temperature ◽  
Vitamin K1 ◽  
Ultrasound Assisted Extraction ◽  
Limit Of Quantification ◽  
Assisted Extraction ◽  
Ultrasound Assisted

Vitamin K1 is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1 to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1 in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1 were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3, v/v) as the elution solvent. Then, vitamin K1 was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2 > 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1 in fat-containing foods.

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

Antioxidants ◽  
2019 ◽  
Vol 8 (8) ◽  
pp. 321 ◽  
Author(s):  
Dandan Wang ◽  
Liangxiao Zhang ◽  
Yueqing Xu ◽  
Xin Qi ◽  
Xuefang Wang ◽  
...  
Keyword(s):  
Response Surface Methodology ◽  
Formic Acid ◽  
Response Surface ◽  
Accurate Determination ◽  
Agricultural Product ◽  
Extraction Temperature ◽  
Ultrasound Assisted Extraction ◽  
Assisted Extraction ◽  
Ultrasound Assisted

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—d-homoproline, vitamin B2, coniferyl aldehyde, hesperidin, phloretin, N-acetyl-l-leucine, l-hyoscyamine, ferulic acid, 5-methoxypsoralen, and 8-methoxypsoralen—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–Burman test, and Box–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 °C, extraction power of 410.0 W, extraction time of 65 min. The total yield of targets was 21.74 μg/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 × 2.1 mm, 3 μm). 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 µg/kg and from 0.04 to 0.34 µg/kg, respectively. The validation results indicated that the method had reasonable linearity (R2 ≥ 0.9990), good recoveries (71.1%–118.3%), satisfactory intra-day precision (≤9.6%) and inter-day precision (≤12.9%), and negligible matrix effects (≤13.8%). This simultaneous quantification method was accurate, fast, and robust for the assessment of sesame nutrition.

scholarly journals Response Surface Optimization of a Rapid Ultrasound-Assisted Extraction Method for Simultaneous Determination of Tetracycline Antibiotics in Manure

2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Lanqing Li ◽  
Mingxing Sun ◽  
Hui Zhou ◽  
Yun Zhou ◽  
Ping Chen ◽  
...  
Keyword(s):  
Response Surface ◽  
Extraction Method ◽  
Extraction Procedure ◽  
Extraction Time ◽  
Extraction Temperature ◽  
Ultrasound Assisted Extraction ◽  
Solution Ph ◽  
Assisted Extraction ◽  
Ultrasound Assisted

A rapid and cleanup-free ultrasound-assisted extraction method is proposed for the simultaneous extraction of oxytetracycline, tetracycline, chlortetracycline, and doxycycline in manure. The analytes were determined using high-performance liquid chromatography with ultraviolet detector. The influence of several variables on the efficiency of the extraction procedure was investigated by single-factor experiments. The temperature, pH, and amount of extraction solution were selected for optimization experiment using response surface methodology. The calibration curves showed good linearity (R2>0.99) for all analytes in the range of 0.1–20 μg/mL. The four antibiotics were successfully extracted from manure with recoveries ranging from 81.89 to 92.42% and good reproducibility (RSD, <4.06%) under optimal conditions, which include 50 mL of McIlvaine buffer extraction solution (pH 7.15) mixed with 1 g of manure sample, extraction temperature of 40°C, extraction time of 10 min, and three extraction cycles. Method quantification limits of 1.75–2.32 mg/kg were obtained for the studied compounds. The proposed procedure demonstrated clear reductions in extraction time and elimination of cleanup steps. Finally, the applicability to tetracyclines antibiotics determination in real samples was evaluated through the successful determination of four target analytes in swine, cow manure, and mixture of animal manure with inorganic fertilizer.

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