High-throughput profiling volatiles in edible oils by cooling assisted solid-phase microextraction technique for sensitive discrimination of edible oils adulteration.

In this study, a cooling assisted solid-phase microextraction technique (CA-SPME) was proposed and used for identifying volatile and semi-volatile compounds in edible oil innovatively coupled to gas chromatography-mass spectrometry. Compared with regular SPME technique, CA-SPME presented significantly higher extraction efficiencies for analytes in edible oil due to its synergistic effect of heating and cooling. After optimization of the extraction conditions including heating temperature, cooling temperature, extraction time, and added amount of edible oil, thirty-eight, thirty-six, twenty-nine, and thirty-three kinds of compounds in peanut oil, olive oil, canola oil, and soybean oil were successfully identified, respectively, using DVB/CAR/PDMS coating with extraction time of 30 min and edible oil amounts of 20 µL. Principal component analysis, partial least squares discriminant analysis, and hierarchical clustering analysis (HCA) were performed to evaluate the potential of proposed method in discriminating edible oils adulteration (peanut oil adulterated with canola oil, peanut oil adulterated with soybean oil, olive oil adulterated with canola oil) subsequently. Results demonstrated that the method was useful in successful discrimination of pure and adulterated edible oils with adulteration percentages ranging from 0.5 to 10%. Furthermore, volatiles contributing to classifications between pure and adulterated edible oils were also illustrated based on variable importance for the projection analysis and distributions of volatiles in HCA heatmaps. The proposed method provided a novel strategy for sensitive detection of edible oil adulteration without any other sample pretreatment.

Determination of Ferulic Acid in Angelica sinensis by Temperature-Controlled Hydrophobic Ionic Liquids-Based Ultrasound/Heating-Assisted Extraction Coupled with High Performance Liquid Chromatography.

Hydrophilic ionic liquids are often used to extract the active ingredients of medicinal plants, while hydrophobic ionic liquids are rarely used to directly extract solid samples. In this paper, a simple, novel and efficient temperature-controlled hydrophobic ionic liquids-based ultrasound/heating-assisted extraction (TC-ILs-UHAE) procedure coupled with high-performance liquid chromatography (HPLC) was developed and applied to the determination of ferulic acid (FA) in Chinese herbal medicine Angelica sinensis. During the extraction procedure, hydrophobic ionic liquids (ILs) were dispersed into water to form cloudy solution (fine droplets) with the aid of ultrasound and heating simultaneous. After extraction, phase separation was easily achieved by centrifuging at 0 °C. Among all ILs used, 1-butyl-3-methylimidazolium bis(trifluoromethanesulphonyl)imide ([C4mim]NTf2) exhibited the highest extraction ability and the possible extraction mechanism was discussed. Additionally, the synergistic effect of heating and ultrasound on the extraction efficiency was investigated. Under the optimized conditions, a good linearity was observed with correlation coefficient (r) of 0.9995. The limit of detection of FA (LOD, S/N = 3) was 9.6 µg/L and the spiked recoveries of FA for real samples were in the range of 91.67 to 102.00% with relative standard deviation (RSD) lower than 3.87%. Compared with the traditional extraction methods, the proposed method gave the highest yield of FA and had the shortest extraction time. Therefore, this method is a potential simple, green and highly efficient technique and expected to be applied to the extraction of other bioactive ingredients in medicinal plants.