离子色谱法测定肥料中三聚氰胺的含量
Determination of Melamine in Fertilizer by IC
摘 要
采用离子色谱分析法检测肥料中三聚氰胺的含量。样品用氨水-甲醇-水(2+7+1)溶液超声振荡提取,离心后经氮气吹干,用3 mmol·L-1甲烷磺酸溶液定容,分离柱和保护柱均为Dionex IonPac R SCS1,淋洗液为含3 mmol·L-1甲烷磺酸的乙腈-水(15+85)。采用非抑制型电导检测器检测。三聚氰胺的线性范围为1.00~1 000 mg·L-1,检出限(3S/N)为5 mg·kg-1,测定下限(9S/N)为15 mg·kg-1。加标回收率在79.3%~116%之间,测定值的相对标准偏差(n=6)在3.4%~13%之间。
三聚氰胺
肥料
Ion chromatography (IC)
Melamine
Fertilizers
Abstract
IC was applied to the determination of melamine in fertilizer. The sample was extracted ultrasonically with a mixture of NH3·H2O+CH3OH+H2O (2+7+1). After centrifuging, the extract was evaporated to dryness by N2-blowing, and the residue was dissolved with 3 mmol·L-1 methylsulfonic acid solution. Dionex IonPac R SCS1 columns were used both as separation and guard columns and a mixture of acetonitrile and 3 mmol·L-1 methylsulphonic acid solution (15+85) was used as eluent. Melamine was detected by non-suppressed conductivity detector. The linearity range of melamine was between 1.00-1 000 mg·L-1. The detection limit was 5 mg·kg-1 and the limit of quantification was 15 mg·kg-1. Values of recovery found by standard addition method were in the range of 79.3%-116% and RSD′s (n=6) were in the range of 3.4%-13%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201512009
所属栏目 工作简报
基金项目 国家质检公益性科研专项基金(201310269)
收稿日期 2014/12/19
修改稿日期
网络出版日期
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备注闵红(1983年-),女,上海人,工程师,主要研究方向为仪器分析。
引用该论文: MIN Hong,SUN Ming-xing,ZHOU Hui,ZHU Zhi-xiu,QIU Feng,ZHANG Ji-dong. Determination of Melamine in Fertilizer by IC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(12): 1670～1674
闵红,孙明星,周辉,朱志秀,邱丰,张继东. 离子色谱法测定肥料中三聚氰胺的含量[J]. 理化检验－化学分册, 2015, 51(12): 1670～1674
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参考文献
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【2】MOSDELLD K, DANIELW H, FREEBORGR P. Melamine and ammeline as nitrogen sources for turfgrasses［J］. Fertilizer Research, 1987,11:79-86.
【3】SOLDALT, NISSEN P. Multiphasic uptake ofamino acids by barley roots［J］. Physiol Plant, 1978,43:181-188.
【4】BOWMAN D C, PAUL JL. Absorption of three slow-release nitrogen fertilizers by perennial ryegrass［J］. Fertilizer Research,1991,29:309-316.
【5】HECKH D, TYL R W. The induction of bladder stones by terephthalic acid, dimethyl terephthalate, and melamine (2,4,6-triaminostriazine) and its relevance to risk assessment［J］. Regul Toxicol Pharmacol, 1985,5(3):294-313.
【6】BAYNESR E, SMITH G, MASON S E,et al. Pharmacokinetics of melamine in pigs following intravenous administration［J］. Food Chem Toxicol, 2008,46(3):1196-1200.
【7】林祥梅,王建峰,贾广乐,等.三聚氰胺的毒性研究［J］.毒理学杂志, 2008,22(3):216-218.
【8】翁文婷,张春.基于三聚氰胺-铜(Ⅱ)-牛血清蛋白络合物的荧光光度法测定饲料中的三聚氰胺［J］.理化检验-化学分册, 2013,49(12):1489-1491.
【9】姜宇,于丽君,吴旭东,等.高效液相色谱法测定饲料中三聚氰胺含量［J］.理化检验-化学分册, 2010,46(6):688-689.
【10】施介华,彭丽.胶束液相色谱法测定乳制品中的三聚氰胺［J］.理化检验-化学分册, 2009,45(12):1369-1372.
【11】孙明星,王亭亭,屠虹,等.土壤中三聚氰胺的高效液相色谱分析［J］.上海交通大学学报:农业科学版, 2012,30(1):29-33.
【12】牛计伟,荆涛,戴晴,等.分子印迹固相萃取-高效液相色谱法用于奶粉样品中痕量三聚氰胺的残留检测［J］.华中科技大学学报:医学版, 2012,41(2):185-189.
【13】杨兴龙,周玮,丁红梅,等.高效液相色谱法测定蛋制品中三聚氰胺［J］.理化检验-化学分册, 2011,47(1):97-98.
【14】GB/T 22288-2008 植物源产品中三聚氰胺、三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸的测定气相色谱-质谱法［S］.
【15】王维,徐颖,张凤娟,等.气相色谱-质谱法检测豆粉中的三聚氰胺［J］.化学分析计量, 2010,19(1):81-82.
【16】吴银良,杨挺,朱勇.气相色谱-质谱法测定土壤中三聚氰胺残留量［J］.分析试验室, 2009,28(12):88-90.
【17】韩冬芳,王德汉,黄培钊,等.三聚氰胺在土壤中的残留及其对大白菜生长的影响［J］.环境科学, 2010,31(3):787-792.
【18】李爱军,张代辉,马书民,等.液相色谱-串联质谱法测定饲料中三聚氰胺残留量［J］.分析化学, 2008,36(5):699-701.
【19】张林田,段建发,林隆强,等.高效液相色谱-串联质谱法测定食品中三聚氰胺［J］.理化检验-化学分册, 2010,46(10):1220-1221.
【20】TIAN Yong-qiang, CHEN Li-ming, GAO Li-hong, et al. Comparison of three methods for detection of melamine in compost and soil［J］. Sci Total Environ, 2012,15:417-418.
【21】TIAN Yong-qiang, CHEN Li-ming, GAO Li-hong, et al. Composting of waste paint sludge containing melamine resin and the compost's effect on vegetable growth and soil water quality［J］. Encironmental Pollution, 2012,162(3):129-137.
【22】刘京生.不用抑制器的新型硅胶阳离子分离柱IonPac SCS1［J］.环境化学, 2005,24(2):229-230.
【23】龚文杰,韩小江,赵立达.非抑制电导阳离子色谱法测定空气中的乙醇胺和三甲胺［J］.中国卫生检验杂质, 2011(10):2397-2398.
【24】赵忠琼,梁隆,陈媛媛.离子色谱法测定高热值混合糖电解质注射液中阴阳离子的含量［J］.药物分析杂志, 2013,32(11):1991-1995.
【25】赵善贞,邓晓军,伊雄海,等.固相萃取-亲水相互作用色谱/串联质谱法同时测定食品中三聚氰胺和三聚氰酸［J］.色谱, 2012,30(7):677-683.
【2】MOSDELLD K, DANIELW H, FREEBORGR P. Melamine and ammeline as nitrogen sources for turfgrasses［J］. Fertilizer Research, 1987,11:79-86.
【3】SOLDALT, NISSEN P. Multiphasic uptake ofamino acids by barley roots［J］. Physiol Plant, 1978,43:181-188.
【4】BOWMAN D C, PAUL JL. Absorption of three slow-release nitrogen fertilizers by perennial ryegrass［J］. Fertilizer Research,1991,29:309-316.
【5】HECKH D, TYL R W. The induction of bladder stones by terephthalic acid, dimethyl terephthalate, and melamine (2,4,6-triaminostriazine) and its relevance to risk assessment［J］. Regul Toxicol Pharmacol, 1985,5(3):294-313.
【6】BAYNESR E, SMITH G, MASON S E,et al. Pharmacokinetics of melamine in pigs following intravenous administration［J］. Food Chem Toxicol, 2008,46(3):1196-1200.
【7】林祥梅,王建峰,贾广乐,等.三聚氰胺的毒性研究［J］.毒理学杂志, 2008,22(3):216-218.
【8】翁文婷,张春.基于三聚氰胺-铜(Ⅱ)-牛血清蛋白络合物的荧光光度法测定饲料中的三聚氰胺［J］.理化检验-化学分册, 2013,49(12):1489-1491.
【9】姜宇,于丽君,吴旭东,等.高效液相色谱法测定饲料中三聚氰胺含量［J］.理化检验-化学分册, 2010,46(6):688-689.
【10】施介华,彭丽.胶束液相色谱法测定乳制品中的三聚氰胺［J］.理化检验-化学分册, 2009,45(12):1369-1372.
【11】孙明星,王亭亭,屠虹,等.土壤中三聚氰胺的高效液相色谱分析［J］.上海交通大学学报:农业科学版, 2012,30(1):29-33.
【12】牛计伟,荆涛,戴晴,等.分子印迹固相萃取-高效液相色谱法用于奶粉样品中痕量三聚氰胺的残留检测［J］.华中科技大学学报:医学版, 2012,41(2):185-189.
【13】杨兴龙,周玮,丁红梅,等.高效液相色谱法测定蛋制品中三聚氰胺［J］.理化检验-化学分册, 2011,47(1):97-98.
【14】GB/T 22288-2008 植物源产品中三聚氰胺、三聚氰酸一酰胺、三聚氰酸二酰胺和三聚氰酸的测定气相色谱-质谱法［S］.
【15】王维,徐颖,张凤娟,等.气相色谱-质谱法检测豆粉中的三聚氰胺［J］.化学分析计量, 2010,19(1):81-82.
【16】吴银良,杨挺,朱勇.气相色谱-质谱法测定土壤中三聚氰胺残留量［J］.分析试验室, 2009,28(12):88-90.
【17】韩冬芳,王德汉,黄培钊,等.三聚氰胺在土壤中的残留及其对大白菜生长的影响［J］.环境科学, 2010,31(3):787-792.
【18】李爱军,张代辉,马书民,等.液相色谱-串联质谱法测定饲料中三聚氰胺残留量［J］.分析化学, 2008,36(5):699-701.
【19】张林田,段建发,林隆强,等.高效液相色谱-串联质谱法测定食品中三聚氰胺［J］.理化检验-化学分册, 2010,46(10):1220-1221.
【20】TIAN Yong-qiang, CHEN Li-ming, GAO Li-hong, et al. Comparison of three methods for detection of melamine in compost and soil［J］. Sci Total Environ, 2012,15:417-418.
【21】TIAN Yong-qiang, CHEN Li-ming, GAO Li-hong, et al. Composting of waste paint sludge containing melamine resin and the compost's effect on vegetable growth and soil water quality［J］. Encironmental Pollution, 2012,162(3):129-137.
【22】刘京生.不用抑制器的新型硅胶阳离子分离柱IonPac SCS1［J］.环境化学, 2005,24(2):229-230.
【23】龚文杰,韩小江,赵立达.非抑制电导阳离子色谱法测定空气中的乙醇胺和三甲胺［J］.中国卫生检验杂质, 2011(10):2397-2398.
【24】赵忠琼,梁隆,陈媛媛.离子色谱法测定高热值混合糖电解质注射液中阴阳离子的含量［J］.药物分析杂志, 2013,32(11):1991-1995.
【25】赵善贞,邓晓军,伊雄海,等.固相萃取-亲水相互作用色谱/串联质谱法同时测定食品中三聚氰胺和三聚氰酸［J］.色谱, 2012,30(7):677-683.
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