富硒蛹虫草中有机硒的分析
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摘要
建立高分辨-连续光源石墨炉原子吸收光谱法(high resolution-continuum source graphite furnace atomic absorption spectrophotometry,HR-CS GFAAS)测定富硒蛹虫草中有机硒的方法。参照DBS42/002-2014《湖北省食品安全地方标准富有机硒食品硒含量要求》制备富硒蛹虫草总硒测定试样,参照GB 1903.21-2016《食品安全国家标准食品营养强化剂富硒酵母》制备富硒蛹虫草无机硒测定试样,再使用HR-CS GFAAS测定富硒蛹虫草总硒和无机硒。试验以Pd(NO_3)_2(1 g/L)和Mg(NO_3)_2(0.5 g/L)混合溶液为基体改进剂,通过试验优化出基体改进剂最佳添加体积为5μL,最佳灰化温度为1 100℃,最佳原子化温度为2 200℃。测定结果表明,富硒蛹虫草总硒含量为1.407 mg/g,无机硒含量为0.083 mg/g,计算出有机硒含量为1.324 mg/g,所占百分比为94.1%,这说明富硒蛹虫草含有丰富的有机硒,是补硒良品。总硒和无机硒的加标回收率分别为95.7%和94.0%,相对标准偏差<4.5%。该方法快速、准确、稳定,具有较高的实用价值,为分析食品中微量元素含量及其形态提供科学依据。
An effective method was developed for the determination of organic selenium in selenium-enriched Cordyceps militaris by high resolution-continuum source graphite furnace atomic absorption spectrophotometry(HR-CS GFAAS). The samples were pretreated according to the standard of DBS42/002-2014 and GB1903.21-2016,respectively. The mixture of Pd(NO_3)_2(1 g/L)and Mg(NO_3)_2(0.5 g/L)was selected as the matrix modifier with the best volume of 5 μL,and the best ashing temperature was 1 100 ℃,the best atomization temperature was 2 200 ℃ by single factor experiments. Further determination of selenium under the condition of the above,the result showed that the total selenium in selenium-enriched cordyceps militaris was 1.407 mg/g,and the inorganic selenium were 0.083 mg/g. The organic selenium in selenium-enriched cordyceps militaris was 1.324 mg/g by calculating,and had reached 94.1 % of total selenium. These indicate that the selenium-enriched cordyceps militaris contain rich organic selenium and are good filling selenium products. The recoveries for total selenium and inorganic selenium were 95.7 % and 94.0 % respectively,relative standard deviation were less than 4.5 %. Therefore,the proposed method was rapid,accurate and stable with a high practical value. It provided scientific basis for analysis of many trace elements and their forms in food.
An effective method was developed for the determination of organic selenium in selenium-enriched Cordyceps militaris by high resolution-continuum source graphite furnace atomic absorption spectrophotometry(HR-CS GFAAS). The samples were pretreated according to the standard of DBS42/002-2014 and GB1903.21-2016,respectively. The mixture of Pd(NO_3)_2(1 g/L)and Mg(NO_3)_2(0.5 g/L)was selected as the matrix modifier with the best volume of 5 μL,and the best ashing temperature was 1 100 ℃,the best atomization temperature was 2 200 ℃ by single factor experiments. Further determination of selenium under the condition of the above,the result showed that the total selenium in selenium-enriched cordyceps militaris was 1.407 mg/g,and the inorganic selenium were 0.083 mg/g. The organic selenium in selenium-enriched cordyceps militaris was 1.324 mg/g by calculating,and had reached 94.1 % of total selenium. These indicate that the selenium-enriched cordyceps militaris contain rich organic selenium and are good filling selenium products. The recoveries for total selenium and inorganic selenium were 95.7 % and 94.0 % respectively,relative standard deviation were less than 4.5 %. Therefore,the proposed method was rapid,accurate and stable with a high practical value. It provided scientific basis for analysis of many trace elements and their forms in food.
引文
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[24]陈安徽,陈尚龙,巫永华,等.黄精酵素口服液中钙、铁和锌的形态分析[J].现代食品科技,2016,32(1):1425-1427
[25]陈琛,苏珂,陈贵堂,等.灰树花中铁的存在形态分析[J].食品科学,2013,34(22):189-192
[2]Zhang Z,Zhao P,Guo J,et al.The extraction of different solubility protein in selenium enriched peanuts and the analysis of their antioxidant activity[J].Science&Technology of Food Industry,2012,33(4):323-326
[3]Bodnar M,Konieczka P.Evaluation of candidate reference material obtained from selenium-enriched sprouts for the purpose of selenium speciation analysis[J].LWT-Food Science and Technology,2016,70:286-295
[4]李红卫,王开萍,吴娱,等.柱前衍生-反相高效液相色谱法研究富硒米曲霉中有机硒形态[J].食品科学,2015,36(22):137-141
[5]Mao G H,Ren Y,Li Q,et al.Anti-tumor and immunomodulatory activity of selenium(Se)-polysaccharide from Se-enriched Grifola frondosa[J].International Journal of Biological Macromolecules,2016,82(10):607-613
[6]Wang Y D,Wang X,Wong Y S.Generation of selenium-enriched rice with enhanced grain yield,selenium content and bioavailability through fertilisation with selenite[J].Food Chemistry,2013,141(3):2385-2393
[7]Bo Y,Wang D,Wei G,et al.Selenium-enriched Candida utilis:Efficient preparation with l-methionine and antioxidant capacity in rats[J].Journal of Trace Elements in Medicine&Biology,2012,27(1):7-11
[8]Gionfriddo E,Naccarato A,Sindona G,et al.A reliable solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry method for the assay of selenomethionine and selenomethylselenocysteine in aqueous extracts:Difference between selenized and not-enriched selenium potatoes[J].Analytica Chimica Acta,2012,747(20):58-66
[9]Mahn A,Zamorano M,Barrientos H,et al.Optimization of a process to obtain selenium-enriched freeze-dried broccoli with high antioxidant properties[J].LWT-Food Science and Technology,2012,47(2):267-273
[10]LIU LIHANG,FAN WANLUN.Incomplete digestion FAAS-faes determination of calcium,magnesium and potassium in human footexuviae[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2005,37(2):348-352
[11]Dong J Z,Ding J,Yu P Z,et al.Composition and distribution of the main active components in selenium-enriched fruit bodies of Cordyceps militaris,link[J].Food Chemistry,2013,137(1/4):164-167
[12]Zhang B,Zhou K,Zhang J,et al.Accumulation and species distribution of selenium in Se-enriched bacterial cells of the Bifidobacterium animalis 01[J].Food Chemistry,2009,115(2):727-734
[13]王欣,幸苑娜,陈泽勇,等.高效液相色谱-电感耦合等离子体质谱法检测富硒食品中6种硒形态[J].分析化学,2013,41(11):1669-1674
[14]杨洋,吴小勇,张湛,等.富硒灵芝发酵培养工艺及产物抗氧化能力研究[J].现代食品科技,2010,26(12):1349-1353
[15]Peronico V C D,Raposo J L.Ultrasound-assisted extraction for the determination of Cu,Mn,Ca,and Mg in alternative oilseed crops using flame atomic absorption spectrometry[J].Food Chemistry,2016,196:1287-1292
[16]Ozbek N,Baysal A.A new approach for the determination of sulphur in food samples by high-resolution continuum source flame atomic absorption spectrometer[J].Food Chemistry,2015,168(168):460-463
[17]Paz-Rodríguez B,Aboal-Somoza M,Bermejo-Barrera P.Application of High Resolution-Continuum Source Flame Atomic Absorption Spectrometry(HR-CS FAAS):Determination of trace elements in tea and tisanes[J].Food Chemistry,2015,170:492-500
[18]J Santos,M T Oliva-Teles,C Delerue-Matos,et al.Multi-elemental analysis of ready-to-eat“baby leaf”vegetables using microwave digestion and high-resolution continuum source atomic absorption spectrometry[J].Food Chemistry,2014,151(151):311-316
[19]Baysal A,Akman S.A practical method for the determination of sulphur in coal samples by high-resolution continuum source flame atomic absorption spectrometry[J].Talanta,2011,85(5):2662-2665
[20]Ozbek N,Akman S.Method development for the determination of fluorine in toothpaste via molecular absorption of aluminum mono fluoride using a high-resolution continuum source nitrous oxide/acetylene flame atomic absorption spectrophotometer[J].Talanta,2012,94(6):246-250
[21]Brandao G C,Jesus R M D,Silva E G P D,et al.Use of slurry sampling for the direct determination of zinc in yogurt by high resolution-continuum source flame atomic absorption spectrometry[J].Talanta,2010,81(4/5):1357-1359
[22]秦杰,陈尚龙,张建萍,等.微波消解-原子吸收法测定鸡精中金属元素[J].食品研究与开发,2014(22):63-67
[23]张建萍,陈尚龙,刘恩岐,等.微波消解-HR-CS AAS法测定几种调味品中的微量元素[J].现代食品科技,2013,29(6):1424-1427
[24]陈安徽,陈尚龙,巫永华,等.黄精酵素口服液中钙、铁和锌的形态分析[J].现代食品科技,2016,32(1):1425-1427
[25]陈琛,苏珂,陈贵堂,等.灰树花中铁的存在形态分析[J].食品科学,2013,34(22):189-192