气相色谱-三重四极杆质谱联用法测定尿样中的碘化物
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摘要
目的建立了尿样中碘化物的2-丁酮衍生化、气相色谱-三重四极杆质谱联用测定方法。方法尿样通过乙酸锌和亚铁氰化钾沉淀蛋白及杂质,在酸性条件下,重铬酸钾氧化碘离子为碘单质,再采用丁酮衍生化,经环己烷萃取衍生物,萃取液经过DB-5MS毛细管色谱柱分离,在多反应监测模式下,使用三重四级杆质谱仪外标峰面积法定量检测。结果碘化物在20μg/L～500μg/L相关系数为0. 999 5,本方法检出限为1. 0μg/L,方法定量下限为5. 0μg/L,平均加标回收率为95. 3%～98. 0%,相对标准偏差为2. 9%～4. 1%。本方法与国家标准检测方法中的砷铈分光光度法(WS/T 107—2006)比较,差异无统计学意义(P> 0. 05),对标准物质进行了分析,结果令人满意。结论本方法简单、快速、灵敏,可以用于尿样中碘化物的测定。
Objective To develop a method for the determination of iodide in urine by gas chromatography-triple quadrupole mass spectrometry after butanone derivatization. Methods Protein and other impurities were first precipitated with zinc acetate and potassium ferrocyanide and then under acidic condition,iodine ions in sample solution were oxidized into iodine with potassium dichromate. Iodide in sample solution was derived with butanone,and then extracted with cyclohexane,and finally separated with DB-5MS capillary column and detected with triple quadrupole mass spectrometer in the multiple reaction monitoring( MRM) mode. The quantification was based on external standard method. Results The concentration of iodide showed good linear relation within 20 μg/L-500 μg/L with the correlation coefficient( r) of 0. 999 5. The detection limit was1. 0 μg/L,and the lowest limit of quantification was 5. 0 μg/L. The average recovery of the method was within 95. 3%-98. 0%,with the relative standard derivations( RSD) of 2. 9%-4. 1%. Compared with As-Ce catalysis spectrophotometry( WS/T 107—2006),the differences were not statistically significant( P > 0. 05). And the analysis results of standard reference materials were satisfactory. Conclusion The method is simple,rapid and sensitive,which is suitable for the routine analysis of iodide in urine samples.
Objective To develop a method for the determination of iodide in urine by gas chromatography-triple quadrupole mass spectrometry after butanone derivatization. Methods Protein and other impurities were first precipitated with zinc acetate and potassium ferrocyanide and then under acidic condition,iodine ions in sample solution were oxidized into iodine with potassium dichromate. Iodide in sample solution was derived with butanone,and then extracted with cyclohexane,and finally separated with DB-5MS capillary column and detected with triple quadrupole mass spectrometer in the multiple reaction monitoring( MRM) mode. The quantification was based on external standard method. Results The concentration of iodide showed good linear relation within 20 μg/L-500 μg/L with the correlation coefficient( r) of 0. 999 5. The detection limit was1. 0 μg/L,and the lowest limit of quantification was 5. 0 μg/L. The average recovery of the method was within 95. 3%-98. 0%,with the relative standard derivations( RSD) of 2. 9%-4. 1%. Compared with As-Ce catalysis spectrophotometry( WS/T 107—2006),the differences were not statistically significant( P > 0. 05). And the analysis results of standard reference materials were satisfactory. Conclusion The method is simple,rapid and sensitive,which is suitable for the routine analysis of iodide in urine samples.
引文
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[12]叶海朋,江阳,周凯. 3-戊酮衍生化-气相色谱法快速检测尿碘含量[J].中国卫生检验杂志,2016,26(10):1393-1395.
[13]曹丽玲,王可,王小青. ICP-MS与砷铈催化分光光度法测定尿中碘的方法对比[J].光谱实验室,2012,29(5):3242-3245.
[14]张钦龙,高舸.带八级杆碰撞/反应池的电感耦合等离子体质谱法测定尿中碘[J].中国卫生检验杂志,2012,22(9):2023-2027.
[15]杨忠乔,吴龙,王小芳.稀氨水稀释-电感耦合等离子体质谱法直接测定尿中碘[J].中国卫生检验杂志,2011,21(6):1375-1377.
[2]管克,詹珍洁,陈建业.瓯海区孕妇尿中碘含量情况调查[J].中国卫生检验杂志,2012,22(11):2740-2745.
[3]沈烨红,卢仁泉,郭林.尿碘测定在甲状腺肿瘤筛查中的临床价值[J].中国肿瘤,2011,20(9):699-702.
[4]中华人民共和国卫生部. WS/T 107—2006尿中碘的砷铈催化分光光度测定方法[S].北京:人民卫生出版社,2006.
[5]严继东,曹丽军.尿碘砷铈催化分光光度测定法的注意事项[J].环境与健康杂志,2008,25(1):48.
[6]张亚平,黄嫣红,李呐,等.尿碘的过硫酸铵消化-低砷量砷铈催化分光光度测定法的化学动力学研究与应用[J].中华地方病学杂志,2013,32(3):318-324.
[7]黄丽,郑莹,黎永艳.尿碘砷铈催化分光光度测定法中影响因素的探讨[J].现代预防医学,2013,40(10):1936-1938.
[8]胡红梅,谢宏斌.过硫酸铵消化测定尿中碘的方法的探讨[J].中国卫生检验杂志,2009,19(9):2169-2174.
[9]迟忠云,孔祥民,常海华.尿中碘的砷铈催化分光光度法的探讨[J].中国地方病防治杂志,2010,25(3):222-223.
[10]赵丹莹,温雅,郭蒙京.离子色谱法快速测定尿碘[J].中国卫生检验杂志,2013,23(7):1725-1728.
[11]高晓宇,崔鹏.催化荧光光度法测定尿碘[J].医学动物防治,2016,32(10):1140-1142.
[12]叶海朋,江阳,周凯. 3-戊酮衍生化-气相色谱法快速检测尿碘含量[J].中国卫生检验杂志,2016,26(10):1393-1395.
[13]曹丽玲,王可,王小青. ICP-MS与砷铈催化分光光度法测定尿中碘的方法对比[J].光谱实验室,2012,29(5):3242-3245.
[14]张钦龙,高舸.带八级杆碰撞/反应池的电感耦合等离子体质谱法测定尿中碘[J].中国卫生检验杂志,2012,22(9):2023-2027.
[15]杨忠乔,吴龙,王小芳.稀氨水稀释-电感耦合等离子体质谱法直接测定尿中碘[J].中国卫生检验杂志,2011,21(6):1375-1377.