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    不同提取方法对红松籽油提取效果及功能性质的影响

    Effects of different extraction methods on extraction effect and functional properties of Korean pine seed oil

    • 摘要:
        目的  立足于溶剂法,通过对比超声波、微波、光波单独处理较短时间的红松籽油的得率,以及处理后单独浸提红松籽油得率的增加情况,明确在红松籽油提取过程中处于主导作用的方法,同时确认4种提取方法对红松籽油的理化指标、脂肪酸和抗氧化能力的影响。
        方法  按照GB/T 5009.229—2016《食品中酸价的测定》、GB/T 5532—2008《动植物油脂 碘值的测定》和GB/T 5009.227—2016《食品中过氧化值的测定》分别测定4种方法提取的红松籽油的酸值、碘值和过氧化物值,采用气相色谱–质谱联用法测定红松籽油中脂肪酸的种类和质量分数,采用分光光度法测定红松籽油对DPPH·和ABTS+·的清除能力。
        结果  正己烷作为最佳提取溶剂,当提取温度25 ℃,液料比18 mL/g,浸提时间5 h红松籽油得率为65.52%。超声波法(300 W,10 min)、微波法(380 W,100 s)、光波法(400 W,11 min)单独处理时的红松籽油得率分别为67.63%、62.26%、58.25%。上述3种方法处理后再单独使用正己烷浸提,使总提取时间达到5 h后的红松籽油得率分别增加了2.18%、4.50%、6.10%。4种方法提取的红松籽油符合GB/T 2716—2018《食品安全国家标准 植物油》中酸值(≤ 4 mg/g)、过氧化值(≤ 0.25 g/100 g)的限量标准。溶剂法制备出的红松籽油的酸值和过氧化值均最低(P < 0.05)。脂肪酸质量分数由高到低分别是亚油酸(44.54% ~ 46.32%)、油酸(28.29 % ~ 28.83%)和皮诺敛酸(13.15% ~ 14.51%)。溶剂法、超声波法、微波法、光波法所提取的红松籽油清除DPPH·和ABTS+·的IC50值分别是9.41、8.80、9.43、9.61 g/L和5.10、5.51、6.10、5.43 g/L。
        结论  对超声波法、微波法和光波法单独作用及浸提后得率进行比较,发现超声波法、微波法和光波法在提取过程中起主导作用。与溶剂法、微波法和光波法相比,超声波法提取的红松籽油得率高,不饱和脂肪酸质量分数高,抗氧化能力强,能够达到较好的提取效果,此方法应用于红松籽制油工业中具有一定优势。

       

      Abstract:
        Objective  Based on solvent method, by comparing the yields of Korean pine seed oil separately treated by ultrasonic method, microwave method or light wave method, and the soaking yields of Korean pine seed oil after separate method treatment, the dominant method in the extraction process of Korean pine seed oil was identified. At the same time, the effects of four extraction methods on physicochemical indexes, fatty acids and antioxidant capacity of Korean pine seed oil were confirmed.
        Method  According to the GB/T 5009.229−2016 Determination of Acid Value in Food, GB/T 5532−2008 Determination of Iodine Value of Animal and Vegetable Oils and GB/T 5009.227−2016 Determination of Peroxide Value in Food, the acid value, iodine value and peroxide value of Korean pine seed oil extracted by the four methods were determined. The type and mass fraction of fatty acids in Korean pine seed oil were determined by gas chromatography-mass spectrometry method, and the scavenging abilities of Korean pine seed oil to DPPH· and ABTS+· were determined by spectrophotometry.
        Result  The optimum extraction solvent was n-hexane. When the extraction temperature was 25 ℃, the liquid to solid ratio was 18 mL/g, the extraction time was 5 h, the yield of Korean pine seed oil was 65.52%. The yield of Korean pine seed oil was 67.63%, 62.26% and 58.25% by ultrasonic (300 W, 10 min), microwave (380 W, 100 s) and light wave (400 W, 11 min), respectively. After the three methods treated separately and the extraction was carried out with n-hexane individually, the yield increased by 2.18%, 4.50% and 6.10%, respectively after the total time reaching 5 h. The Korean pine seed oil extracted by the four methods can meet the limit standard of acid value (≤ 4 mg/g) and peroxide value (≤ 0.25 g/100 g) in GB/T 2716−2018 National Food Safety Standard Vegetable Oil. The acid value and peroxide value of Korean pine seed oil prepared by organic solvent method were the lowest (P < 0.05). The mass fractions of fatty acid from high to low were linoleic acid (44.54% − 46.32%), oleic acid (28.29% − 28.83%) and pinocyanic acid (13.15% − 14.51%). The DPPH· and ABTS+· IC50 values of Korean pine seed oil extracted by solvent, ultrasonic, microwave and light wave methods were 9.41, 8.80, 9.43, 9.61 g/L and 5.10, 5.51, 6.10, 5.43 g/L, respectively.
        Conclusion  The yields of ultrasonic method, microwave method or light wave method separately, and soaking yields after the single treatment were compared. It is found that ultrasonic, microwave and light wave method play a leading role in the extraction process. Compared with the solvent method, microwave method and light wave method, Korean pine seed oil extracted by the ultrasonic method has a higher extraction percentage, a higher mass fraction of unsaturated fatty acid, a stronger antioxidant capacity, and can achieve better extraction effect. This method has some advantages in the Korean pine seed oil extraction industry.

       

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