微波辅助萃取结合LC-ICP/MS法测定食品中无机砷
|
摘要
建立了一种微波辅助萃取的前处理技术,应用于食品中无机砷的测定。方法选用0. 15 mol/L HNO3作为提取液,并加入H2O2,80℃微波辅助萃取20 min,采用LC-ICP/MS对食品中无机砷含量进行测定。结果表明:在此条件下,H2O2可将亚砷酸盐[As(III)]完全氧化成砷酸盐[As(V)],从而分离出峰时间重合的亚砷酸盐和有机砷。无机砷在0. 05～1. 0 mg/kg范围内线性关系良好,相关系数大于0. 999,方法检出限为0. 02 mg/kg,定量限为0. 05 mg/kg,加标回收率为96. 0%～104. 2%,相对标准偏差为1. 8%～2. 9%。应用本方法对食品分析水平评估计划(FAPAS)质控样品蟹肉罐头和大米样品中无机砷进行测定,测定结果与其证书的参考值相符。方法适用于食品中无机砷含量的检测。
A microwave-assisted extraction pretreatment technique was established in this study for inorganic arsenic determination in food. 0. 15 mol/L nitric acid with addition of hydrogen peroxide was chosen as the extract solution. Microwave-assisted extraction was performed at 80°C for 20 min. The inorganic arsenic content in food was determined by liquid chromatography-inductively coupled plasma mass spectrometry( LC-ICP/MS). The results showed that hydrogen peroxide can completely oxidize arsenite [As( III) ] to arsenate [As( V) ] in this way. Then arsenite and organic arsenic with peak time overlap can be separated. The inorganic arsenic had good linearity in the range of 0. 05-1. 0 mg/kg. The correlation coefficient was > 0. 999. The limit of detection was 0. 02 mg/kg and the limit of quantification was 0. 05 mg/kg. The recovery rates of standard addition was 96. 0%-104. 2%,and the relative standard deviations were 1. 8%-2. 9%. Quality control canned crab meat and rice samples were bought from Food Analysis Performance Assessment Scheme( FAPAS). The method was used to determine the inorganic arsenic in real samples. Compared to the reference value of the FAPAS certificate,the results were accurate. The method is efficient and accurate,and suitable for the detection of inorganic arsenic in foods. It has a high application value in inorganic arsenic determination in aquatic products and algae foods.
A microwave-assisted extraction pretreatment technique was established in this study for inorganic arsenic determination in food. 0. 15 mol/L nitric acid with addition of hydrogen peroxide was chosen as the extract solution. Microwave-assisted extraction was performed at 80°C for 20 min. The inorganic arsenic content in food was determined by liquid chromatography-inductively coupled plasma mass spectrometry( LC-ICP/MS). The results showed that hydrogen peroxide can completely oxidize arsenite [As( III) ] to arsenate [As( V) ] in this way. Then arsenite and organic arsenic with peak time overlap can be separated. The inorganic arsenic had good linearity in the range of 0. 05-1. 0 mg/kg. The correlation coefficient was > 0. 999. The limit of detection was 0. 02 mg/kg and the limit of quantification was 0. 05 mg/kg. The recovery rates of standard addition was 96. 0%-104. 2%,and the relative standard deviations were 1. 8%-2. 9%. Quality control canned crab meat and rice samples were bought from Food Analysis Performance Assessment Scheme( FAPAS). The method was used to determine the inorganic arsenic in real samples. Compared to the reference value of the FAPAS certificate,the results were accurate. The method is efficient and accurate,and suitable for the detection of inorganic arsenic in foods. It has a high application value in inorganic arsenic determination in aquatic products and algae foods.
引文
[1] Kim JY,Kim W I,Kunhikrishnan A,Kang,Kim D H,Lee Y J,Kim Y J,Kim C T. Food Sci. Biotechnol.,2013,22(6):1509
[2] Xu J J,Feng X,Tang J,Hu Q H,Zhao L Y. J. Food Saf. Qual.,2016,7(6):2153胥佳佳,冯鑫,汤静,胡秋辉,赵立艳.食品安全质量检测学报,2016,7(6):2153
[3] Chen B W,Le X. Chris. Environ. Chem.,2011,30(11):1936陈保卫,Le X Chris.环境化学,2011,30(11):1936
[4] GB 2762-2017,National food safety standard-Maximum levels of contaminants in foods GB 2762-2017,食品安全国家标准食品中污染物限量
[5] Yang Q,Fan Y M,Yang M Y,Gong J,He Z Z,Guan Z B,Zeng Y,Deng Y Z. Food Sci. Technol.,2015,40(7):338杨庆,樊亚鸣,杨敏仪,龚剑,何芝洲,关灼斌,曾源,邓亚中.食品科技,2015,40(7):338
[6] Du J,Ma J H,Zhang Q,Sun B,Huang J,Shen H. Marin. Fish.,2015,37(5):465杜晶,马家海,张勤,孙彬,黄健,沈辉.海洋渔业,2015,37(5):465
[7] Wang Y,Zhang C H,Ge Y. Chin. J. Anal. Lab.,2013,32(5):34王亚,张春华,葛滢.分析试验室,2013,32(5):34
[8] Lu Y N,Wei J H,Xu K,Zhang L T,Chen J W. Phys. Test. Chem. Anal. B,2017,53(9):1087陆奕娜,魏建华,许慨,张林田,陈建伟.理化检验:化学分册,2017,53(9):1087
[9] Yuan L. Chin. J. Anal. Lab.,2017,36(8):975苑蕾.分析试验室,2017,36(8):975
[10] Llorente-Mirandes T,Barbero M,Rubio R,Lopez-Sanchez J F. Food Chem.,2014,158(8):207
[11] Che D S,Zhang F J,Du J J. Environ. Chem.,2014,33(7):1130车东昇,张建锋,杜晶晶.环境化学,2014,33(7):1130
[12] Wei C J,Xu H,Liu J X,Han H. Agric. Qual. Std.,2007(s1):43韦昌金,徐浩,刘霁欣,韩昊.农业质量标准,2007(s1):43
[13] Wu C Y,Qian Z Z,Wu S H,Cao A Y,Liu Z Y,Liu S J. J. Fujian Fish.,2010,3(1):29吴成业,钱卓真,吴抒怀,曹爱英,刘智禹,刘淑集.福建水产,2010,3(1):29
[14] GB/T 23372-2009,Determination of inorganic arsenic in food-Liquid chromatography-inductively coupled plasma mass spectrometry GB/T 23372-2009,食品中无机砷的测定液相色谱-电感耦合等离子体质谱法
[15] GB 5009. 11-2014,National food safety standard-Determination of total arsenic and inorganic arsenic in food GB 5009. 11-2014,食品安全国家标准食品中总砷及无机砷的测定
[2] Xu J J,Feng X,Tang J,Hu Q H,Zhao L Y. J. Food Saf. Qual.,2016,7(6):2153胥佳佳,冯鑫,汤静,胡秋辉,赵立艳.食品安全质量检测学报,2016,7(6):2153
[3] Chen B W,Le X. Chris. Environ. Chem.,2011,30(11):1936陈保卫,Le X Chris.环境化学,2011,30(11):1936
[4] GB 2762-2017,National food safety standard-Maximum levels of contaminants in foods GB 2762-2017,食品安全国家标准食品中污染物限量
[5] Yang Q,Fan Y M,Yang M Y,Gong J,He Z Z,Guan Z B,Zeng Y,Deng Y Z. Food Sci. Technol.,2015,40(7):338杨庆,樊亚鸣,杨敏仪,龚剑,何芝洲,关灼斌,曾源,邓亚中.食品科技,2015,40(7):338
[6] Du J,Ma J H,Zhang Q,Sun B,Huang J,Shen H. Marin. Fish.,2015,37(5):465杜晶,马家海,张勤,孙彬,黄健,沈辉.海洋渔业,2015,37(5):465
[7] Wang Y,Zhang C H,Ge Y. Chin. J. Anal. Lab.,2013,32(5):34王亚,张春华,葛滢.分析试验室,2013,32(5):34
[8] Lu Y N,Wei J H,Xu K,Zhang L T,Chen J W. Phys. Test. Chem. Anal. B,2017,53(9):1087陆奕娜,魏建华,许慨,张林田,陈建伟.理化检验:化学分册,2017,53(9):1087
[9] Yuan L. Chin. J. Anal. Lab.,2017,36(8):975苑蕾.分析试验室,2017,36(8):975
[10] Llorente-Mirandes T,Barbero M,Rubio R,Lopez-Sanchez J F. Food Chem.,2014,158(8):207
[11] Che D S,Zhang F J,Du J J. Environ. Chem.,2014,33(7):1130车东昇,张建锋,杜晶晶.环境化学,2014,33(7):1130
[12] Wei C J,Xu H,Liu J X,Han H. Agric. Qual. Std.,2007(s1):43韦昌金,徐浩,刘霁欣,韩昊.农业质量标准,2007(s1):43
[13] Wu C Y,Qian Z Z,Wu S H,Cao A Y,Liu Z Y,Liu S J. J. Fujian Fish.,2010,3(1):29吴成业,钱卓真,吴抒怀,曹爱英,刘智禹,刘淑集.福建水产,2010,3(1):29
[14] GB/T 23372-2009,Determination of inorganic arsenic in food-Liquid chromatography-inductively coupled plasma mass spectrometry GB/T 23372-2009,食品中无机砷的测定液相色谱-电感耦合等离子体质谱法
[15] GB 5009. 11-2014,National food safety standard-Determination of total arsenic and inorganic arsenic in food GB 5009. 11-2014,食品安全国家标准食品中总砷及无机砷的测定