快速微波消解-ICP-MS法测定面粉中铝含量
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摘要
目的建立快速微波消解-电感耦合等离子体质谱(ICP-MS)法测定面粉中铝含量的准确测定方法。方法针对面粉中本底铝难以消解问题,本研究系统优化了微波消解体系、消解温度、消解时间等参数,采用硝酸-氢氟酸作为消解体系,200℃微波消解1.5 h后200℃赶酸,赶干后立即加入5%硝酸溶液加热复溶10 min,用1%硝酸定容至25 ml,采用ICP-MS法检测面粉中铝含量。结果标准物质河南小麦(GBW 10046)中铝的测定结果符合给定的标准值,证明经优化的前处理方案能有效消解出面粉中的本底铝。铝的方法检出限为0.023 mg/kg,加标回收率为98.4%～101.0%,精密度为2.4%～4.1%。结论采用文中方法可以彻底消解面粉中难溶性和结合态铝,从而可准确测定面粉中铝含量。该方法安全快速,精密度好,准确度高。
Objective To establish an accurate method for the rapid determination of aluminum in flour by ICP-MS coupled with microwave digestion. Methods In order to solve the problem that the background aluminum in flour is difficult to digest, parameters including the microwave digestion system, digestion temperature, and digestion time were optimized in this study. Nitric acid-hydrofluoric acid mixture was used as a digestion system. Flour sample was firstly digested at 200 ℃ for 1.5 h, and then the acid in digestive solution was evaporated at 200 ℃. After completely removing the hydrofluoric acid in digestive solution, 5% nitric acid in water was added and heated for 10 minutes, and then it was diluted to 25 ml with 1% nitric acid aqueous solution. The aluminum content in flour was determined by ICP-MS. Results The determination results of aluminum in the standard substance Henan wheat(GBW 10046) using the developed method were very close to the given value, proving that the optimized method can effectively extract the background aluminum in flour sample. The limit of detection(LOD) of aluminum was 0.023 mg/kg, while the recovery ranged from 98.4% to 101.0%, with RSD in range of 2.4%-4.1%. Conclusion The developed method in this study can drastically extract the insoluble and bonded aluminum in flour sample and accurate aluminum content can be determined in flour. The proposed method is safe, rapid, precise, and accurate.
Objective To establish an accurate method for the rapid determination of aluminum in flour by ICP-MS coupled with microwave digestion. Methods In order to solve the problem that the background aluminum in flour is difficult to digest, parameters including the microwave digestion system, digestion temperature, and digestion time were optimized in this study. Nitric acid-hydrofluoric acid mixture was used as a digestion system. Flour sample was firstly digested at 200 ℃ for 1.5 h, and then the acid in digestive solution was evaporated at 200 ℃. After completely removing the hydrofluoric acid in digestive solution, 5% nitric acid in water was added and heated for 10 minutes, and then it was diluted to 25 ml with 1% nitric acid aqueous solution. The aluminum content in flour was determined by ICP-MS. Results The determination results of aluminum in the standard substance Henan wheat(GBW 10046) using the developed method were very close to the given value, proving that the optimized method can effectively extract the background aluminum in flour sample. The limit of detection(LOD) of aluminum was 0.023 mg/kg, while the recovery ranged from 98.4% to 101.0%, with RSD in range of 2.4%-4.1%. Conclusion The developed method in this study can drastically extract the insoluble and bonded aluminum in flour sample and accurate aluminum content can be determined in flour. The proposed method is safe, rapid, precise, and accurate.
引文
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[12] 王冰,邵爱梅,夏俊鹏,等.铝的样品处理方法研究[J].食品安全质量检测学报,2016,7(5):27-29.
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[14] 樊祥,韩丽,伊熊海,等.电感耦合等离子体质谱法测定面制食品中铝[J].理化检验:化学分册,2010,46(10):1132-1134.
[15] 候韬乔,孔舒.电感耦合等离子体质谱法测定面制食品中铝含量[J].中国公共卫生管理,2012,28(3):376-377.
[2] 李青,刘思洁,方赤光.食品中铝含量及其危害研究进展[J].食品安全质量检测学报,2016,7(1):14-19.
[3] 张婵,王洪彬,申梅桂.食品中铝的测定及超标对人体的危害[J].光谱实验室,2013,30(2):746-750.
[4] 付晓苹,许玉艳,宋怿,等.食品添加剂和污染物中铝的风险评估[J].中国农学通报,2014,30(30):310-320.
[5] 中华人民共和国卫生和计划生育委员会.GB 2760—2014 食品添加剂使用标准[S].北京:中国标准出版社,2015.
[6] 中华人民共和国卫生和计划生育委员会.GB 5009.182—2017食品中铝的测定[S].北京:中国标准出版社,2017.
[7] 中华人民共和国卫生和计划生育委员会.GB 5009.268—2016食品中多元素的测定[S].北京:中国标准出版社,2017.
[8] 赵立凡,唐宏兵,吴英,等.ICP-MS法测定面制食品中的铝含量[J].环境卫生学杂志,2013,3(3):245-247.
[9] 刘淑君,平庆杰,黄雪琳,等.微波消解样品-电感耦合等离子体质谱法测定面制食品中铝[J].理化检验:化学分册,2012,48(9):1030-1032,1036.
[10] 彭寨玉,李月欢,郑慧华,等.微波消解-电感耦合等离子体质谱法测定面制食品中铝[J].中国卫生检验杂志,2009,19(12):2837-2839.
[11] 李晨光,钱立新.面制食品中铝测定前处理方法的研究与改进[J].中国卫生工程学,2015,14(1):27-29.
[12] 王冰,邵爱梅,夏俊鹏,等.铝的样品处理方法研究[J].食品安全质量检测学报,2016,7(5):27-29.
[13] 裘立晓,徐奋奋,汪娌娜.食品中铝测定前处理方法比较[J].中国卫生检验杂志,2011,21(4):842-843.
[14] 樊祥,韩丽,伊熊海,等.电感耦合等离子体质谱法测定面制食品中铝[J].理化检验:化学分册,2010,46(10):1132-1134.
[15] 候韬乔,孔舒.电感耦合等离子体质谱法测定面制食品中铝含量[J].中国公共卫生管理,2012,28(3):376-377.