超声辅助热水提取-离子色谱法同时测定蔬菜中的硫氰酸盐和高氯酸盐
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摘要
建立同时测定蔬菜中硫氰酸盐和高氯酸盐的离子色谱分析方法。样品采用纯水超声辅助提取,离心后直接过膜的前处理技术,然后采用IonPac AS16离子分析柱进行分离,电导检测器进行检测,KOH溶液梯度洗脱,通过外标法定量。结果表明,硫氰酸盐和高氯酸盐分别在0.2～5.0和0.04～1.00 mg/L范围内具有良好的线性关系,相关系数分别为0.9997和0.9989,检出限分别为0.005、0.008 mg/L,方法回收率分别为89.9%～98.4%和81.2%～94.4%,重复性实验的相对标准偏差分别为1.6%和6.9%。实际样品测定中,8类蔬菜样品全检出一定量的硫氰酸盐和高氯酸盐,其中胡萝卜干的硫氰酸盐和高氯酸盐最高。
A method was developed to determine thiocyanate and perchlorate in vegetables. The sample was extracted by ultrasonic assisted with ultrapure water and filtered after centrifugation as pre-treatment technology.Then the samples were separated with an IonPac AS16 anion analysis column by gradient elution with KOH solution,detected by conductivity detector,and quantified by external standard method. The results showed that,the calibration curve of thiocyanate and perchlorate was linear in the range of 0.2～5.0 mg/L and 0.04～1.00 mg/L with correlation coefficients of 0.9997 and 0.9989,respectively. The limits of quantitation were 0.005,0.008 mg/L,respectively. The recoveries were in the range of 89.9%～98.4% and 81.2%～94.4%,and relative standard deviations repeatability test were 1.6% and 6.9%,respectively. In the result, vegetable samples all contained a certain amount of thiocyanate and perchlorate,and the highest content of carrots dry.
A method was developed to determine thiocyanate and perchlorate in vegetables. The sample was extracted by ultrasonic assisted with ultrapure water and filtered after centrifugation as pre-treatment technology.Then the samples were separated with an IonPac AS16 anion analysis column by gradient elution with KOH solution,detected by conductivity detector,and quantified by external standard method. The results showed that,the calibration curve of thiocyanate and perchlorate was linear in the range of 0.2～5.0 mg/L and 0.04～1.00 mg/L with correlation coefficients of 0.9997 and 0.9989,respectively. The limits of quantitation were 0.005,0.008 mg/L,respectively. The recoveries were in the range of 89.9%～98.4% and 81.2%～94.4%,and relative standard deviations repeatability test were 1.6% and 6.9%,respectively. In the result, vegetable samples all contained a certain amount of thiocyanate and perchlorate,and the highest content of carrots dry.
引文
[1]顾欣,黄士新,李丹妮,等.乳中硫氰酸盐对人类健康的风险评估[J]. 中国兽药杂志,2010,44(9):45-49.
[2]臧海军,张克英. 菜籽饼粕中硫代葡萄糖苷的危害与脱毒措施研究[J]. 饲料工业,2007,28(2):62-64.
[3]廖静,谷浩,牟文,等. 硫氰酸钠对斑马鱼毒性的评价[J]. 生态毒理学报,2011,6(1):43-47.
[4]Lijinsky W,kovatch R.Chronic toxicity tests of sodium thiocyanate with sodium nitrite in F344 rats[J].Toxicology and Industrial Health,1989,5(1):25-29.
[5]吴剑平,张鑫,顾欣,等. 上海生鲜牛乳中硫氰酸钠生理浓度调查及主要影响因素研究[J]. 中国乳品工业,2014,42(6):19-22.
[6]张格祥,王海军,王蕾蕾,等. 白菜、豆角对大鼠90天喂养试验研究[J]. 中国食物与营养,2012,18(12):69-73.
[7]陈基耘. 离子色谱法测定乳品中硫氰酸钠含量[J]. 化学分析计量,2014,23(4):42-44.
[8]李红敏,陈霞,王静,等. 离子色谱法测定乳及乳制品中硫氰酸根含量[J].食品研究与开发,2015,36(7):78-81.
[9]张丽宏,黄晓林,鄂来明,等. 分光光度法测定乳及乳粉中的硫氰酸钠[J]. 中国乳品工业,2016,44(7):41-43.
[10]廖振宇,汪晓冬.离子色谱法检测乳制品中硫氰酸根含量[J].食品研究与开发,2014,35(10):89-91.
[11]Niemann R A,Anderson D L.Determination of iodide and thiocyanate in powdered milk and infant formula by on-line enrichment ion chromatography with photodiode array detection[J]. Journal of Chromatography A,2008,1200(2):193-197.
[12]张遴,王文瑞,蔡砚,等. 分光光度法测定婴幼儿食品中硫氰酸钠[J]. 理化检验(化学分册),2013,49:717-719.
[13]Backus S M,Klawuun P,Brown S,et al.Determination of perchlorate in selected surface waters in the Great Lakes Basin byHPLC/MS/MS[J]. Chemosphere,2005,61(6):834-843.
[14]Shi Y L,Zhang N,Gao J M,et al. Effect of fireworks display on perchlorate in air aerosols during the Spring Festival[J]. Atmospheric Environment,201l,45(6):1323-1327.
[15]吴春笃,李顺,许小红,等. 高氯酸盐的环境毒理学效应及其机制的研究进展[J]. 环境与健康杂志,2013,30(1):85-89.
[16]Krynitsky A J,Niemann R A,Nortrup D A. Determination of perchlorate anion in foods by ion chromatography tandem mass spectrometry[J]. Analytical Chemistry,2004,76(18):5518-5522.
[17]Dyke J V,Kirka B,Martinelango K,et al.Sample processing method for the determination of perchlorate in milk[J].Analytica Chimica Acta,2006,567(1):73-78.
[18]刘小芳,方从容,刘慧,等. 离子色谱-串联质谱法检测茶叶中的高氯酸盐[J]. 色谱,2016,34(10):986-988.
[19]Aribih E,Le Blanc Y J C,Antonsen S,et al. Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry(IC-ESI MS/MS)[J]. Analytica Chimica Acta,2006,567(1):39-47.
[20]Furdui V I,Tomassini F. Trends and sources of perchlorate in Arctic snow[J]. Environmental Science and Technology,2010,44(2):588-592.
[21]钱蜀,谢永洪,杨坪,等. 离子色谱-串联质谱测定地表水中高氯酸盐[J]. 中国环境监测,2014,30(3):125-131.
[22]高峰,刘岩,孔维恒,等. 离子色谱-质谱测定碳酸饮料中的亚氯酸盐、氯酸盐和高氯酸盐[J]. 食品科学,2013,34(22):261-264.
[23]Gu B H,Ruan C M,Wang W. Perchlorate detection at nanomolar concentrations by surface-enhanced Raman scattering[J]. Applied Spectroscopy,2009,63(1):98-102.
[24]王飞,高飞,崔宗岩,等. 离子色谱法测定乳粉中的高氯酸盐[J]. 中国无机分析化学,2017,7(3):8-11.
[25]李柚,喻宏伟,王飞,等. 离子色谱法测定葡萄酒中的高氯酸盐[J]. 色谱,2016,34(10):989-991.
[26]宇盛好,李亦奇,张旭晟,等. 上海市市售食品中高氯酸盐污染的暴露评估[J].上海预防医学,2017,29(6):426-430.
[27]邵琳智,吴映璇,欧阳少伦,等. 离子交换高效液相色谱-串联质谱法测定鸡肉和鸡肝中的高氯酸盐[J]. 食品科学,2016,37(20):167-171.
[28]李静,王雨,梁立娜. 离子色谱法同时分析奶粉中碘离子和硫氰酸根[J].分析实验室,2010,29(5):17-20.
[2]臧海军,张克英. 菜籽饼粕中硫代葡萄糖苷的危害与脱毒措施研究[J]. 饲料工业,2007,28(2):62-64.
[3]廖静,谷浩,牟文,等. 硫氰酸钠对斑马鱼毒性的评价[J]. 生态毒理学报,2011,6(1):43-47.
[4]Lijinsky W,kovatch R.Chronic toxicity tests of sodium thiocyanate with sodium nitrite in F344 rats[J].Toxicology and Industrial Health,1989,5(1):25-29.
[5]吴剑平,张鑫,顾欣,等. 上海生鲜牛乳中硫氰酸钠生理浓度调查及主要影响因素研究[J]. 中国乳品工业,2014,42(6):19-22.
[6]张格祥,王海军,王蕾蕾,等. 白菜、豆角对大鼠90天喂养试验研究[J]. 中国食物与营养,2012,18(12):69-73.
[7]陈基耘. 离子色谱法测定乳品中硫氰酸钠含量[J]. 化学分析计量,2014,23(4):42-44.
[8]李红敏,陈霞,王静,等. 离子色谱法测定乳及乳制品中硫氰酸根含量[J].食品研究与开发,2015,36(7):78-81.
[9]张丽宏,黄晓林,鄂来明,等. 分光光度法测定乳及乳粉中的硫氰酸钠[J]. 中国乳品工业,2016,44(7):41-43.
[10]廖振宇,汪晓冬.离子色谱法检测乳制品中硫氰酸根含量[J].食品研究与开发,2014,35(10):89-91.
[11]Niemann R A,Anderson D L.Determination of iodide and thiocyanate in powdered milk and infant formula by on-line enrichment ion chromatography with photodiode array detection[J]. Journal of Chromatography A,2008,1200(2):193-197.
[12]张遴,王文瑞,蔡砚,等. 分光光度法测定婴幼儿食品中硫氰酸钠[J]. 理化检验(化学分册),2013,49:717-719.
[13]Backus S M,Klawuun P,Brown S,et al.Determination of perchlorate in selected surface waters in the Great Lakes Basin byHPLC/MS/MS[J]. Chemosphere,2005,61(6):834-843.
[14]Shi Y L,Zhang N,Gao J M,et al. Effect of fireworks display on perchlorate in air aerosols during the Spring Festival[J]. Atmospheric Environment,201l,45(6):1323-1327.
[15]吴春笃,李顺,许小红,等. 高氯酸盐的环境毒理学效应及其机制的研究进展[J]. 环境与健康杂志,2013,30(1):85-89.
[16]Krynitsky A J,Niemann R A,Nortrup D A. Determination of perchlorate anion in foods by ion chromatography tandem mass spectrometry[J]. Analytical Chemistry,2004,76(18):5518-5522.
[17]Dyke J V,Kirka B,Martinelango K,et al.Sample processing method for the determination of perchlorate in milk[J].Analytica Chimica Acta,2006,567(1):73-78.
[18]刘小芳,方从容,刘慧,等. 离子色谱-串联质谱法检测茶叶中的高氯酸盐[J]. 色谱,2016,34(10):986-988.
[19]Aribih E,Le Blanc Y J C,Antonsen S,et al. Analysis of perchlorate in foods and beverages by ion chromatography coupled with tandem mass spectrometry(IC-ESI MS/MS)[J]. Analytica Chimica Acta,2006,567(1):39-47.
[20]Furdui V I,Tomassini F. Trends and sources of perchlorate in Arctic snow[J]. Environmental Science and Technology,2010,44(2):588-592.
[21]钱蜀,谢永洪,杨坪,等. 离子色谱-串联质谱测定地表水中高氯酸盐[J]. 中国环境监测,2014,30(3):125-131.
[22]高峰,刘岩,孔维恒,等. 离子色谱-质谱测定碳酸饮料中的亚氯酸盐、氯酸盐和高氯酸盐[J]. 食品科学,2013,34(22):261-264.
[23]Gu B H,Ruan C M,Wang W. Perchlorate detection at nanomolar concentrations by surface-enhanced Raman scattering[J]. Applied Spectroscopy,2009,63(1):98-102.
[24]王飞,高飞,崔宗岩,等. 离子色谱法测定乳粉中的高氯酸盐[J]. 中国无机分析化学,2017,7(3):8-11.
[25]李柚,喻宏伟,王飞,等. 离子色谱法测定葡萄酒中的高氯酸盐[J]. 色谱,2016,34(10):989-991.
[26]宇盛好,李亦奇,张旭晟,等. 上海市市售食品中高氯酸盐污染的暴露评估[J].上海预防医学,2017,29(6):426-430.
[27]邵琳智,吴映璇,欧阳少伦,等. 离子交换高效液相色谱-串联质谱法测定鸡肉和鸡肝中的高氯酸盐[J]. 食品科学,2016,37(20):167-171.
[28]李静,王雨,梁立娜. 离子色谱法同时分析奶粉中碘离子和硫氰酸根[J].分析实验室,2010,29(5):17-20.
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