高效液相色谱-电感耦合等离子体质谱法测定食品中的六价铬含量
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摘要
目的建立高效液相色谱-电感鍋合等离子体质谱法(high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry, HPLC-ICP/MS)测定食品中六价铬含量,同时间接测定三价铬含量。方法总铬采用总铬采用国标GB 5009.268-2016中的第一法进行测定。样品中六价铬经0.1 mol/L的磷酸氢二钾溶液(pH 7.9～8.1)提取溶液中的铬酸根离子,高效液相色谱分离,ICP-MS检测。三价铬含量可以通过总铬减去六价铬含量得到。结果六价铬在质量浓度0.4～10.0μg/L范围内,呈良好的线性关系,方法检出限为0.03 mg/kg,加标回收率为91.0%～106%(n=8),相对标准偏差为2.8%～4.9%(n=8)。结论该方法的提取条件保持了六价铬原始形态不变,操作简单,灵敏度高,重现性好,适合食品中六价铬含量的定量检测。
Objective To establish a method for determination the hexavalent chromium content in the food by high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP/MS), and to indirectly determine the trivalent chromium content at the same time. Methods Total chromium was determined by the first method in national standard GB 5009.268-2016. Chromium(VI) in sample was extracted by 0.1 mol/L dipotassium hydrogen phosphate solution(pH 7.9～8.1), separated with HPLC and detected by ICP-MS. Chromium(III) content could be obtained by subtracting the chromium(VI) content from the total chromium content. Results The linear relationship of chromium(VI) was obtained in the range of 0.4-10.0 μg/L, and the limit of detection was 0.03 mg/kg. Recoveries and relative standard deviations were 91.0%-106% and 2.8%-4.9%(n=8), respectively. Conclusion The extraction conditions of this method keep the original form of chromium(VI), it is simple, sensitivity, good reproducibility, and can applied in the quantitative determination of chromium(VI) in foods.
Objective To establish a method for determination the hexavalent chromium content in the food by high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP/MS), and to indirectly determine the trivalent chromium content at the same time. Methods Total chromium was determined by the first method in national standard GB 5009.268-2016. Chromium(VI) in sample was extracted by 0.1 mol/L dipotassium hydrogen phosphate solution(pH 7.9～8.1), separated with HPLC and detected by ICP-MS. Chromium(III) content could be obtained by subtracting the chromium(VI) content from the total chromium content. Results The linear relationship of chromium(VI) was obtained in the range of 0.4-10.0 μg/L, and the limit of detection was 0.03 mg/kg. Recoveries and relative standard deviations were 91.0%-106% and 2.8%-4.9%(n=8), respectively. Conclusion The extraction conditions of this method keep the original form of chromium(VI), it is simple, sensitivity, good reproducibility, and can applied in the quantitative determination of chromium(VI) in foods.
引文
[1]周利英,周锦帆,左鹏飞.六价铬和三价铬的检测技术[J].化学通报,2013, 76(10):915-922.Zhou L, Zhou JF, Zuo PF. Detection technology for Cr(VI)and Cr(Ⅲ)[J].Chemistry, 2013, 76(10):915-922.
[2]刘明理,曹进,丁宏,等.液相色谱-质谱法测定保健食品中三价铬及六价铬含量[J].食品安全质量检测学报,2017, 8(7):2465-2470.Liu ML, Cao J, Ding H, et al. Determination of trivalent and hexavalent chromium in healthy food by liquid chromatography-mass spectrometry[J]. J Food Saf Qual, 2017, 8(7):2465-2470.
[3] SN/T 2210-2008保健食品中六价铬的测定-离子色谱电感耦合等离子体质谱法[S].SN/T 2210-2008 Determination of hexavalent chromium in health foods IC-ICP/MS method[S].
[4] ISO 17075-2:2017皮革中六价铬含量的检测[S].ISO 17075-2:2017 Chemical determination of chromium(Ⅵ)content in leather[S].
[5] GB/T 17593.3-2006纺织品重金属的测定第3部分:六价铬分光光度法[S].GB/T 17593.3-2006 Textiles determination of heavy metals Part 3:Hexavalent chromium spectrophotometric method[S].
[6]杨振宇,郭德华,杨克成,等.保健食品中的六价铬测定[J].质谱学报,2008, 29(2):92-96.Yang ZY, Guo DH, Yang KC, et al. Determination of hexavalent chromium in health foods[J]. J Chin Mass Spectrom Soc, 2008, 29(2):92-96.
[7]倪张林,汤富彬,屈明华,等.微波灰化-液相色谱-电感耦合等离子体质谱联用测定干食用菌中的三价铬和六价铬[J].色谱,2014, 32(2):174-178.Ni ZL, Tang FH, Qu MH, et al. Determination of trivalent chromium and hexavalent chromium in dried edible fungi by microwave ashing-liquid chromatography with inductively coupled plasma mass spectrometry[J].Chin J Chromatogr, 2014, 32(2):174-178.
[8]郭少飞,王鹏,王帆,等.高效液相色谱-电感耦合等离子体质谱法测定粉质化妆品中的六价铬[J].检验检疫学刊,2012, 22(4):8-13.Guo SF, Wang P, Wang F, et al. Determination of chromium(VI)in silty cosmetics using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Inspect Quarant, 2012, 22(4):8-13.
[9]禄春强.液相色谱-电感耦合等离子体质谱法测定水嘴中六价铬和三价铬析出量[J].分析测试学报,2017, 35(12):1639-1642.Lu CQ. Determination of chromium(VI)and chromium(Ⅲ)stripped from stopcock by liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Instrum Anal, 2017, 35(12):1639-1642.
[10]张冀飞,高欣,杨晓兵.高效液相色谱-电感耦合等离子体质谱联用测定儿童玩具中痕量铬(Ⅲ)与铬(Ⅵ)[J].分析测试学报,2015, 34(2):232-236.Zhang JF, Gao X, Yang XB. Determination of chromium(Ⅲ)and(Ⅵ)in children's toys using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Instrum Anal, 2015, 34(2):232-236.
[11]刀谞,吕怡兵,滕恩江,等.离子色谱-电感耦合等离子体质谱联用测定大气颗粒物PM_(2.5)和PM_(10)中的六价铬[J].色谱,2014, 32(9):936-941.Dao X, Lu YB, Teng EJ, et al. Determi nation of hexavalent chromium in atmospheric particles PM_(2.5)and PM_(10)by ion chromatography with inductively coupled plasma mass spectrometry[J]. Chin J Chromatogr,2014, 32(9):936-941.
[12] Stanislawska M, Janasik B, Wasowicz W. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP-MS)for determination of chromium compounds in the air at the workplace[J]. Talanta, 21014, 12:14-19.
[13]杨振宇,郭德华.离子色谱法测定食品中的六价铬[J].分析试验室,2005,24(增刊):148.Yang ZY, Guo DH. Detemination of hexavalent chromium by ion chromatography[J]. Chin J Anal Lab, 2005, 24(Supplement):148.
[14] Frederick T,Stanin.在环境中六价铬的迁移与固定[J].铬盐工业,2010,1:16-47.Frederick T, Stanin. Migration and fixaltion of Cr(VI)in environment[J].Chromic Salt Ind, 2010, 1:16-47.
[15]樊祥,曹晨,张润何,等.全自动微波消解-电感耦合等离子体质谱法测定保健品食中12种常量、微量元素[J].分析试验室,2018, 37(2):157-162.Fan X, Cao C, Zhang RH, et al. Determination of 12 major and trace elements in health-care products with microwave assisted full-automatic sample digestion-inductively coupled plasma mass spectrometry[J]. Chin J Anal Lab, 2018, 37(2):157-162.
[16]邵惟俊.汞、镉、钛、铬化合物的Eh-pH图[J].长安大学学报:地球科学版,1980:30-38.Shao WJ. Eh-pH diagrams of mercury, cadmium, titanium and chromium compounds[J]. J Chang'an Unive:Earth Sci, 1980:30-38.
[17] GB 5009.268-2016食品中多元素的测定[S].GB 5009.268-2016 Determination of muilti-elements in foods[S].
[2]刘明理,曹进,丁宏,等.液相色谱-质谱法测定保健食品中三价铬及六价铬含量[J].食品安全质量检测学报,2017, 8(7):2465-2470.Liu ML, Cao J, Ding H, et al. Determination of trivalent and hexavalent chromium in healthy food by liquid chromatography-mass spectrometry[J]. J Food Saf Qual, 2017, 8(7):2465-2470.
[3] SN/T 2210-2008保健食品中六价铬的测定-离子色谱电感耦合等离子体质谱法[S].SN/T 2210-2008 Determination of hexavalent chromium in health foods IC-ICP/MS method[S].
[4] ISO 17075-2:2017皮革中六价铬含量的检测[S].ISO 17075-2:2017 Chemical determination of chromium(Ⅵ)content in leather[S].
[5] GB/T 17593.3-2006纺织品重金属的测定第3部分:六价铬分光光度法[S].GB/T 17593.3-2006 Textiles determination of heavy metals Part 3:Hexavalent chromium spectrophotometric method[S].
[6]杨振宇,郭德华,杨克成,等.保健食品中的六价铬测定[J].质谱学报,2008, 29(2):92-96.Yang ZY, Guo DH, Yang KC, et al. Determination of hexavalent chromium in health foods[J]. J Chin Mass Spectrom Soc, 2008, 29(2):92-96.
[7]倪张林,汤富彬,屈明华,等.微波灰化-液相色谱-电感耦合等离子体质谱联用测定干食用菌中的三价铬和六价铬[J].色谱,2014, 32(2):174-178.Ni ZL, Tang FH, Qu MH, et al. Determination of trivalent chromium and hexavalent chromium in dried edible fungi by microwave ashing-liquid chromatography with inductively coupled plasma mass spectrometry[J].Chin J Chromatogr, 2014, 32(2):174-178.
[8]郭少飞,王鹏,王帆,等.高效液相色谱-电感耦合等离子体质谱法测定粉质化妆品中的六价铬[J].检验检疫学刊,2012, 22(4):8-13.Guo SF, Wang P, Wang F, et al. Determination of chromium(VI)in silty cosmetics using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Inspect Quarant, 2012, 22(4):8-13.
[9]禄春强.液相色谱-电感耦合等离子体质谱法测定水嘴中六价铬和三价铬析出量[J].分析测试学报,2017, 35(12):1639-1642.Lu CQ. Determination of chromium(VI)and chromium(Ⅲ)stripped from stopcock by liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Instrum Anal, 2017, 35(12):1639-1642.
[10]张冀飞,高欣,杨晓兵.高效液相色谱-电感耦合等离子体质谱联用测定儿童玩具中痕量铬(Ⅲ)与铬(Ⅵ)[J].分析测试学报,2015, 34(2):232-236.Zhang JF, Gao X, Yang XB. Determination of chromium(Ⅲ)and(Ⅵ)in children's toys using high performance liquid chromatography-inductively coupled plasma mass spectrometry[J]. J Instrum Anal, 2015, 34(2):232-236.
[11]刀谞,吕怡兵,滕恩江,等.离子色谱-电感耦合等离子体质谱联用测定大气颗粒物PM_(2.5)和PM_(10)中的六价铬[J].色谱,2014, 32(9):936-941.Dao X, Lu YB, Teng EJ, et al. Determi nation of hexavalent chromium in atmospheric particles PM_(2.5)and PM_(10)by ion chromatography with inductively coupled plasma mass spectrometry[J]. Chin J Chromatogr,2014, 32(9):936-941.
[12] Stanislawska M, Janasik B, Wasowicz W. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry(HPLC-ICP-MS)for determination of chromium compounds in the air at the workplace[J]. Talanta, 21014, 12:14-19.
[13]杨振宇,郭德华.离子色谱法测定食品中的六价铬[J].分析试验室,2005,24(增刊):148.Yang ZY, Guo DH. Detemination of hexavalent chromium by ion chromatography[J]. Chin J Anal Lab, 2005, 24(Supplement):148.
[14] Frederick T,Stanin.在环境中六价铬的迁移与固定[J].铬盐工业,2010,1:16-47.Frederick T, Stanin. Migration and fixaltion of Cr(VI)in environment[J].Chromic Salt Ind, 2010, 1:16-47.
[15]樊祥,曹晨,张润何,等.全自动微波消解-电感耦合等离子体质谱法测定保健品食中12种常量、微量元素[J].分析试验室,2018, 37(2):157-162.Fan X, Cao C, Zhang RH, et al. Determination of 12 major and trace elements in health-care products with microwave assisted full-automatic sample digestion-inductively coupled plasma mass spectrometry[J]. Chin J Anal Lab, 2018, 37(2):157-162.
[16]邵惟俊.汞、镉、钛、铬化合物的Eh-pH图[J].长安大学学报:地球科学版,1980:30-38.Shao WJ. Eh-pH diagrams of mercury, cadmium, titanium and chromium compounds[J]. J Chang'an Unive:Earth Sci, 1980:30-38.
[17] GB 5009.268-2016食品中多元素的测定[S].GB 5009.268-2016 Determination of muilti-elements in foods[S].