天然富硒植物无花果叶中硒提取方法的研究
|
摘要
本试验旨在比较天然富硒植物无花果叶中硒的提取方法。试验采用4种方法从无花果叶中提取硒,分别是混合酸消解法、超声-微波协同萃取法、索氏提取法和磁力搅拌法,讨论每种方法的不同提取条件对提取效果的影响,并将提取到的硒用灵敏度高的荧光光度法进行定量。结果表明:1)混合酸消解法提取硒的效果最好,超声-微波协同萃取法提取效果略次之,磁力搅拌法提取硒的效果最差。2)混合酸消解法4种不同的混合酸消解体系中,高氯酸-硫酸-硝酸(体积比1∶1∶3)组成的消解体系提取硒的效果最好,消解24 h提取硒的含量为0.13μg/g。3)正交试验确定超声-微波协同萃取法的最佳提取条件是用甲醇作为提取剂,微波功率400 W,提取时间15 min,物料比1∶10 (g∶mL),在此条件下提取硒的含量为0.12μg/g。由此可知,不同方法提取无花果叶中硒的效果不同。混合酸消解法虽然提取硒的效果最好,但是该方法中用的强酸危险性大,试验周期长;超声-微波协同萃取法提取硒的效果仅略差于混合酸消解法,同时该方法可实时监控,操作简单安全,且试验耗时远远低于混合酸消解法。因此,建议采用超声-微波协同萃取法提取无花果叶中的硒。
This experiment was conducted to compare the extraction method of selenium from fig leaves which had rich selenium as a natural plant. The four extraction methods,including mixed acid digestion method,ultrasound-microwave synergistic extraction method,Soxhlet extraction method and magnetic stirring method were discussed and evaluated. The different conditions for extraction efficiency were optimized and selenium content in fig leaves was measured by fluorescence spectrometry with high sensitivity. The results showed as follows: 1) the mixed acid digestion method had the highest extraction efficiency,the ultrasound-microwave synergistic extraction method was slightly worse than the mixed acid digestion method,and the magnetic stirring method was the worst. 2) In the four different acid digestion systems of mixed acid digestion method,the system consisting of the volume ratio of perchloric acid,sulphuric acid and nitric acid was 1∶ 1∶ 3 had the best effect for extracting selenium. The content of selenium in fig leaves was 0.13 μg/g with extraction time 24 h.3) The content of selenium was 0.12 μg/g with ultrasound-microwave synergistic extraction method. The optimum extraction conditions of ultrasound-microwave synergistic extraction method through orthogonal test were identified as the follows: methanol as solvent,microwave power 400 W,extraction time 15 min and solid-liquid ratio as 1 ∶ 10 (g ∶ mL). The results indicated that there are differences of extraction effect with different methods. The mixed acid digestion method has the best extraction effect but strong acids used in the experiment is too dangerous for the operation with long time digestion. The extraction effect of ultrasound-microwave synergistic extraction method is slightly worse than the mixed acid digestion method,but it can shorten extraction time,reduce sample consumption,operate expediently and monitor in real time. Therefore,ultrasound-microwave synergistic extraction method for extracting selenium from fig leaves is recommended.
This experiment was conducted to compare the extraction method of selenium from fig leaves which had rich selenium as a natural plant. The four extraction methods,including mixed acid digestion method,ultrasound-microwave synergistic extraction method,Soxhlet extraction method and magnetic stirring method were discussed and evaluated. The different conditions for extraction efficiency were optimized and selenium content in fig leaves was measured by fluorescence spectrometry with high sensitivity. The results showed as follows: 1) the mixed acid digestion method had the highest extraction efficiency,the ultrasound-microwave synergistic extraction method was slightly worse than the mixed acid digestion method,and the magnetic stirring method was the worst. 2) In the four different acid digestion systems of mixed acid digestion method,the system consisting of the volume ratio of perchloric acid,sulphuric acid and nitric acid was 1∶ 1∶ 3 had the best effect for extracting selenium. The content of selenium in fig leaves was 0.13 μg/g with extraction time 24 h.3) The content of selenium was 0.12 μg/g with ultrasound-microwave synergistic extraction method. The optimum extraction conditions of ultrasound-microwave synergistic extraction method through orthogonal test were identified as the follows: methanol as solvent,microwave power 400 W,extraction time 15 min and solid-liquid ratio as 1 ∶ 10 (g ∶ mL). The results indicated that there are differences of extraction effect with different methods. The mixed acid digestion method has the best extraction effect but strong acids used in the experiment is too dangerous for the operation with long time digestion. The extraction effect of ultrasound-microwave synergistic extraction method is slightly worse than the mixed acid digestion method,but it can shorten extraction time,reduce sample consumption,operate expediently and monitor in real time. Therefore,ultrasound-microwave synergistic extraction method for extracting selenium from fig leaves is recommended.
引文
[1]SURAI P F,FISININ V I.Selenium in poultry breeder nutrition:an update[J].Animal Feed Science and Technology,2014,191:1-15.
[2]CAO C Y,ZHAO X,FAN R F,et al.Dietary selenium increases the antioxidant levels and ATPase activity in the arteries and veins of poultry[J].Biological Trace Element Research,2016,172(1):222-227.
[3]SURAI P F,KOCHISH I I,FISININ V I,et al.Selenium in poultry nutrition:from sodium selenite to organic selenium sources[J].The Journal of Poultry Science,2018,55(2):79-93.
[4]ZIA W M,KHALIQUE A,NAVEED S,et al.Organic and inorganic selenium in poultry:a review[J].Indian Journal of Animal Research,2018,52(4):483-489.
[5]王登峰.有机硒对奶牛产奶性能、营养物质消化及血液生化指标的影响[D].硕士学位论文.呼和浩特:内蒙古农业大学,2011:33-35.
[6]RAN L W,WU X S,SHEN X Z,et al.Effects of selenium form on blood and milk selenium concentrations,milk component and milk fatty acid composition in dairy cow s[J].Journal of the Science of Food and Agriculture,2010,90(13):2214-2219.
[7]KARKOODI K,CHAMANI M,BEHESHTI M,et al.Effect of organic zinc,manganese,copper,and selenium chelates on colostrum production and reproductive and lameness indices in adequately supplemented holstein cow s[J].Biological Trace Element Research,2012,146(1):42-46.
[8]GUYOT H,SPRING P,ANDRIEU S,et al.Comparative responses to sodium selenite and organic selenium supplements in Belgian Blue cow s and calves[J].Livestock Science,2007,111(3):259-263.
[9]李明,哈斯,介晓磊,等.富含硒钴锌的苜蓿青干草在牛羊饲喂中的效果[J].家畜生态学报,2011,32(4):34-37.
[10]权群学,陈少谋,胡登明.利用天然富硒玉米生产富硒鸡蛋试验[J].黑龙江畜牧兽医,2016(12):106-107.
[11]郭孝,胡华锋,介晓磊,等.日粮中添加富硒钴苜蓿草粉对家兔饲料转化率和肉品质的影响[J].家畜生态学报,2017,38(12):29-33.
[12]吴国杰,舒绪刚,尹国强,等.硒饲料添加剂在动物养殖中的应用[J].广东饲料,2015,24(9):27-29.
[13]释凯,李勇,任大喜,等.有机硒对奶牛生产性能的影响及富硒乳制品开发研究[J].中国畜牧杂志,2015,51(24):44-48.
[14]覃爱苗,唐平,余卫平.硒在植物中的生物学效应[J].东北农业大学学报,2011,42(10):6-11.
[15]刘云,谢锦忠,屈明华,等.湿法消解-原子荧光法测定竹笋中的微量硒[J].竹子研究汇刊,2007,26(3):12-15.
[16]LIU Z Z,GU H Y,YANG L.An approach of ionic liquids/lithium salts based microw ave irradiation pretreatment follow ed by ultrasound-microw ave synergistic extraction for tw o coumarins preparation from Cortex fraxini[J].Journal of Chromatography A,2015,1417:8-20.
[17]YANG Y Q,CHU G H,ZHOU G J,et al.Rapid determination of the volatile components in tobacco by ultrasound-microw ave synergistic extraction coupled to headspace solid-phase microextraction w ith gas chromatography-mass spectrometry[J].Journal of Separation Science,2016,39(6):1173-1181.
[18]TANG S R,SONG H,CHEN Y J,et al.Synergistic extraction and antioxidant activities of ginger polyphenols by ultrasound w ave and microw ave[J].Advanced M aterials Research,2012,550-553:580-585.
[19]OCHOA-RIVAS A,NAVA-VALDEZ Y,SERNA-SALDVAR S O,et al.M icrow ave and ultrasound to enhance protein extraction from peanut flour under alkaline conditions:effects in yield and functional properties of protein isolates[J].Food and Bioprocess Technology,2017,10(3):543-555.
[20]XU W,YAN X H,SHAO R,et al.Optimization of ultrasonic-microw ave synergistic extraction of ricinine from castor cake by response surface methodology[J].Current Pharmaceutical Biotechnology,2016,17(13):1126-1133.
[2]CAO C Y,ZHAO X,FAN R F,et al.Dietary selenium increases the antioxidant levels and ATPase activity in the arteries and veins of poultry[J].Biological Trace Element Research,2016,172(1):222-227.
[3]SURAI P F,KOCHISH I I,FISININ V I,et al.Selenium in poultry nutrition:from sodium selenite to organic selenium sources[J].The Journal of Poultry Science,2018,55(2):79-93.
[4]ZIA W M,KHALIQUE A,NAVEED S,et al.Organic and inorganic selenium in poultry:a review[J].Indian Journal of Animal Research,2018,52(4):483-489.
[5]王登峰.有机硒对奶牛产奶性能、营养物质消化及血液生化指标的影响[D].硕士学位论文.呼和浩特:内蒙古农业大学,2011:33-35.
[6]RAN L W,WU X S,SHEN X Z,et al.Effects of selenium form on blood and milk selenium concentrations,milk component and milk fatty acid composition in dairy cow s[J].Journal of the Science of Food and Agriculture,2010,90(13):2214-2219.
[7]KARKOODI K,CHAMANI M,BEHESHTI M,et al.Effect of organic zinc,manganese,copper,and selenium chelates on colostrum production and reproductive and lameness indices in adequately supplemented holstein cow s[J].Biological Trace Element Research,2012,146(1):42-46.
[8]GUYOT H,SPRING P,ANDRIEU S,et al.Comparative responses to sodium selenite and organic selenium supplements in Belgian Blue cow s and calves[J].Livestock Science,2007,111(3):259-263.
[9]李明,哈斯,介晓磊,等.富含硒钴锌的苜蓿青干草在牛羊饲喂中的效果[J].家畜生态学报,2011,32(4):34-37.
[10]权群学,陈少谋,胡登明.利用天然富硒玉米生产富硒鸡蛋试验[J].黑龙江畜牧兽医,2016(12):106-107.
[11]郭孝,胡华锋,介晓磊,等.日粮中添加富硒钴苜蓿草粉对家兔饲料转化率和肉品质的影响[J].家畜生态学报,2017,38(12):29-33.
[12]吴国杰,舒绪刚,尹国强,等.硒饲料添加剂在动物养殖中的应用[J].广东饲料,2015,24(9):27-29.
[13]释凯,李勇,任大喜,等.有机硒对奶牛生产性能的影响及富硒乳制品开发研究[J].中国畜牧杂志,2015,51(24):44-48.
[14]覃爱苗,唐平,余卫平.硒在植物中的生物学效应[J].东北农业大学学报,2011,42(10):6-11.
[15]刘云,谢锦忠,屈明华,等.湿法消解-原子荧光法测定竹笋中的微量硒[J].竹子研究汇刊,2007,26(3):12-15.
[16]LIU Z Z,GU H Y,YANG L.An approach of ionic liquids/lithium salts based microw ave irradiation pretreatment follow ed by ultrasound-microw ave synergistic extraction for tw o coumarins preparation from Cortex fraxini[J].Journal of Chromatography A,2015,1417:8-20.
[17]YANG Y Q,CHU G H,ZHOU G J,et al.Rapid determination of the volatile components in tobacco by ultrasound-microw ave synergistic extraction coupled to headspace solid-phase microextraction w ith gas chromatography-mass spectrometry[J].Journal of Separation Science,2016,39(6):1173-1181.
[18]TANG S R,SONG H,CHEN Y J,et al.Synergistic extraction and antioxidant activities of ginger polyphenols by ultrasound w ave and microw ave[J].Advanced M aterials Research,2012,550-553:580-585.
[19]OCHOA-RIVAS A,NAVA-VALDEZ Y,SERNA-SALDVAR S O,et al.M icrow ave and ultrasound to enhance protein extraction from peanut flour under alkaline conditions:effects in yield and functional properties of protein isolates[J].Food and Bioprocess Technology,2017,10(3):543-555.
[20]XU W,YAN X H,SHAO R,et al.Optimization of ultrasonic-microw ave synergistic extraction of ricinine from castor cake by response surface methodology[J].Current Pharmaceutical Biotechnology,2016,17(13):1126-1133.