婴幼儿米粉中磷含量测定方法的探讨
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摘要
比较及建立检测婴幼儿米粉中磷含量的方法。参考GB 5009.87—2016"食品安全国家标准食品中磷的测定"的方法,比较湿法消解-钒钼酸铵法、干法消解-钒钼酸铵法、微波消解-钒钼酸铵法以及微波消解-ICP法对婴幼儿米粉中磷含量的测定结果。结果表明,分别采用湿法消解、干法消解和微波消解前处理样品,经钒钼酸铵法对标准物质各进行6次测定,测定均值分别为265.506,266.608和274.072 mg/100 g,三者差异不显著(p>0.05),且微波消解-钒钼酸铵法测定食品中磷标准曲线线性范围为:0~25μg/m L(r=0.999 9),其样品在加标浓度1.40~4.92 mg/g范围下测得加标回收率为96.29%~109.41%,精密度为2.0%(N=6),方法检出限为1.470 mg/100 g。另外,微波消解-钒钼酸铵法较微波消解-ICP法数据准确。微波消解-钒钼酸铵法准确、快速,重复性好,并且得出该方法适合于婴幼儿米粉中磷含量测定。
The method of the content of phosphorus in infant rice flour was compared and established. The method of GB 5009.87—2016 "National Food Safety Standard Determination of Phosphorus in Foods" was adopted. The results of the content of phosphorus in the samples treated by wet digestion-ammonium vanadate method, dry digestion-ammonium vanadate method and microwave digestion-vanadium molybdate method were compared. The results of samples were digested by wet digestion and microwave digestion. The mean values of the standard substances were 265.506, 266.608 and 274.072 mg/100 g, respectively. There was no significant difference(p>0.05) about them. The latter measured results about the calibration curve were linear in the range of 0-25 μg/m L(r=0.999 9). The recoveries were 96.29%-109.41% in the range of 1.40-4.92 mg/g, and the precision was 2.0%(N=6). The detection limit was 1.470 mg/100 g. In addition, the microwave digestion-vanadium molybdate method was more accurate than microwave digestion-ICP. Microwave digestion-ammonium molybdate method was accurate, rapid and reproducible, and could be used for the determination of phosphorus in infant rice flour.
The method of the content of phosphorus in infant rice flour was compared and established. The method of GB 5009.87—2016 "National Food Safety Standard Determination of Phosphorus in Foods" was adopted. The results of the content of phosphorus in the samples treated by wet digestion-ammonium vanadate method, dry digestion-ammonium vanadate method and microwave digestion-vanadium molybdate method were compared. The results of samples were digested by wet digestion and microwave digestion. The mean values of the standard substances were 265.506, 266.608 and 274.072 mg/100 g, respectively. There was no significant difference(p>0.05) about them. The latter measured results about the calibration curve were linear in the range of 0-25 μg/m L(r=0.999 9). The recoveries were 96.29%-109.41% in the range of 1.40-4.92 mg/g, and the precision was 2.0%(N=6). The detection limit was 1.470 mg/100 g. In addition, the microwave digestion-vanadium molybdate method was more accurate than microwave digestion-ICP. Microwave digestion-ammonium molybdate method was accurate, rapid and reproducible, and could be used for the determination of phosphorus in infant rice flour.
引文
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[22]SZYDLOWSKA-CZERNIAK A,SZLYK E.Spectrophotometric determination of total phosphorus in rape seeds and oils at various stages of technological process:Calculation of phospholipids and non-hydratable phospholipids contents in rapeseed oil[J].Food Chemistry,2003(81):613-619.
[23]HANRAHAN G,SALMASSI T M,KHACHIKIAN C S,et al.Reduced inorganic phosphorus in the natural environment:Significance,speciation and determination[J].Talanta,2005,66(12):435-444.
[24]WU P,ZHAO T,TIAN J C.Phytic acid contents of wheat flours from different mill streams[J].Agricultural Sciences in China,2010,9(11):1684-1688.
[2]李则均,刘滨青.高蛋白大米粉中磷含量测定[J].中国食物与营养,2012,18(5):52-54.
[3]段建坤,杨永,曾爱民.奶粉及大豆制品中磷的形态分析[J].光谱实验室,2012,29(6):3645-3648.
[4]胡彩霞,胡文辉,刘美霞.奶粉中磷含量与储存时间的研究[J].中国食品工业,2012(9):70-71.
[5]俞凌云,赵甜甜,王书园.磷在环境和食品中的测定方法的研究进展[J].江苏调味副食品,2008,25(4):26-31.
[6]谭和平,张玉兰,高杨,等.ICP-AES法在茶叶磷和硫分析中的应用[J].中国测试,2011,37(5):50-52.
[7]谢永洪,张新申,杨坪,等.分光光度法测定磷酸盐的研究进展[J].皮革科学与工程,2009,19(2):35-41.
[8]万益群,吴世芳.超声波提取-等离子体原子发射光谱测定何首乌中的磷脂[J].南昌大学学报(理科版),2007,31(4):348-350.
[9]郭岚,谢明勇,鄢爱平,等.电感耦合等离子体发射光谱法测定植物油中的磷[J].分析实验室,2007,26(4):58-61.
[10]万军红,邵丽华.微波消解:磷钼蓝分光光度法测定奶粉中的磷[J].卫生研究,2009,38(5):617-618.
[11]陆建平,彭剑,石建荣,等.甲基异丁酮萃取-间接火焰原子吸收光谱法测定锑锭中磷[J].冶金分析,2008,28(12):38-40.
[12]刘玉玲.干法灰化-ICP法测定食品中的磷[J].食品工程,2014(2):58-60.
[13]卫敏,LIU RUIHAI,DING LIANG,等.食品中磷的检测方法[J].中国科学(化学),2010,40(7):914-921.
[14]鲁琳,高燕红,胡曙光,等.食品中磷含量检测方法探讨[J].华南预防医学,2012,38(3):58-60.
[15]俞凌云,赵甜甜,王书园.磷在环境和食品中的测定方法的研究进展[J].江苏调味副食品,2008,25(4):26-31.
[16]陈志娟,蔡梦华,高素虹.食品中磷测定方法研究[J].预防医学论坛,2009,12(15):1204-1207.
[17]中华人民共和国卫生部.食品安全国家标准:婴幼儿食品和乳品中磷的测定:GB 5413.22—2010[S].北京:中国标准出版社,2010.
[18]中华人民共和国卫生部.食品安全国家标准:婴儿配方食品:GB 10765—2010[S].北京:中国标准出版社,2010.
[19]中华人民共和国卫生部.食品安全国家标准:较大婴儿和幼儿配方食品:GB 10767—2010[S].北京:中国标准出版社,2010.
[20]中华人民共和国卫生部.食品中磷的测定:GB/T5009.87—2003[S].北京:中国标准出版社,2003.
[21]LOPEZ-GARCIA I,VINAS P,ROMERO-ROMERO R,et al.Fast determination of phosphorus in honey,milk and infant formulas by electrothermal atomic absorption spectrometry using a slurry sampling procedure[J].Spectrochim Acta Part B,2007(62):48-55.
[22]SZYDLOWSKA-CZERNIAK A,SZLYK E.Spectrophotometric determination of total phosphorus in rape seeds and oils at various stages of technological process:Calculation of phospholipids and non-hydratable phospholipids contents in rapeseed oil[J].Food Chemistry,2003(81):613-619.
[23]HANRAHAN G,SALMASSI T M,KHACHIKIAN C S,et al.Reduced inorganic phosphorus in the natural environment:Significance,speciation and determination[J].Talanta,2005,66(12):435-444.
[24]WU P,ZHAO T,TIAN J C.Phytic acid contents of wheat flours from different mill streams[J].Agricultural Sciences in China,2010,9(11):1684-1688.