亲水作用色谱-串联质谱法测定婴幼儿乳粉中的牛磺酸
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摘要
目的:建立婴幼儿乳粉中牛磺酸直接测定的亲水作用色谱-串联质谱(HILIC-MS/MS)检测方法。方法:样品经提取后,采用乙腈和10 mmol/L甲酸铵(0.05%甲酸)作为流动相进行梯度洗脱,质谱在负离子模式下采用多反应监测(MRM),对牛磺酸进行定量测定。结果:牛磺酸在10～200 ng/mL浓度范围线性关系良好,相关系数r为0.9997,检出限为0.04 mg/kg,回收率在81.2～90.5%之间,相对标准偏差小于4.0%。结论:该方法快速、准确、灵敏度高,可用于婴幼儿乳粉中中牛磺酸的直接测定。
Objective:To establish a direct determination method of taurine in infant milk powder by hydrophilic interaction chromatography-mass spectrometry(HILIC-MS/MS). Method:After extraction,acetonitrile and 10 mmol/L ammonium formate(0.05% formic acid)were used as the mobile phase for gradient elution,mass spectrometry was used for quantitative determination of taurine in the negative ion mode by multiple reaction monitoring(MRM). Results:The linear relationship was good in the range of 10～200 ng/mL,and the correlation coefficient was 0.9997,the detection limit was 0.04 mg/kg,the recoveries were 81.2%～90.5%,and the relative standard deviations were less than 4.0%. Conclusion:The method was rapid,accurate and sensitive,and could be applied to the direct determination of taurine in infant milk powder.
Objective:To establish a direct determination method of taurine in infant milk powder by hydrophilic interaction chromatography-mass spectrometry(HILIC-MS/MS). Method:After extraction,acetonitrile and 10 mmol/L ammonium formate(0.05% formic acid)were used as the mobile phase for gradient elution,mass spectrometry was used for quantitative determination of taurine in the negative ion mode by multiple reaction monitoring(MRM). Results:The linear relationship was good in the range of 10～200 ng/mL,and the correlation coefficient was 0.9997,the detection limit was 0.04 mg/kg,the recoveries were 81.2%～90.5%,and the relative standard deviations were less than 4.0%. Conclusion:The method was rapid,accurate and sensitive,and could be applied to the direct determination of taurine in infant milk powder.
引文
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[11]王洪健,周兴起,冯志强,等.氨基酸自动分析仪测定食品中牛磺酸的方法建立[J].现代食品科技,2012,28(3):348-350.
[12]蔡梅,吉文亮,刘华良,等.氨基酸自动分析仪对食品中牛磺酸快速测定方法研究[J].中国卫生检验杂质,2013,23(1):41-45.
[13]张婷,陈雷,刘芸,等.高效液相色谱-高分辨质谱法测定乳粉中的牛磺酸[J].食品安全质量检测学报,2017,8(6):2086-2089.
[14]康明芹,陈明岩,王岸英,等.高效液相色谱-串联质谱法测定保健食品中牛磺酸[J].理化检验(化学分册),2018,54(2):153-155.
[15]邵金良,杨东顺,王丽,等. 固相萃取-高效液相色谱法同时测定牛奶中13种磺胺残留[J].分析实验室,2014,33(11):1322-1325.
[16]朱慧,李克,翟云霞.血清蛋白质组学研究中乙腈沉淀法去除清蛋白的实验研究[J].临床检验杂志,2011(1):16-18.
[17]刘晓云,陈笑艳,钟大放.液相色谱-串联质谱生物分析方法的基质效应和对策[J].质谱学报,2017,38(4):388-399.
[2]中华人民共和国国家卫生和计划生育委员会.GB5009.169-2016食品安全国家标准食品中牛磺酸的测定[S]. 北京:中国标准出版社,2016.
[3]杨涓,魏智清,庞伟,等.分光光度法测定宁夏枸杞中的牛磺酸含量[J].农业科学研究,2005,26(2):28-30.
[4]黄丽丹,邢亚东,王玲玲,等. 2,4-二硝基氟苯柱前衍生化 HPLC 法测定保健食品中牛磺酸含量[J].药物分析杂志,2016,36(1):171-175.
[5]陈申如,胡阳,倪辉,等.高效液相色谱法测定牡蛎中牛磺酸含量[J].中国食品学报,2013,13(2):193-198.
[6]王芬,张婷,顾振新,等.高效液相色谱法测定紫菜中牛磺酸含量[J].食品科学,2012,33(18):162-164.
[7]邹晓莉,黎源倩,曾红燕,等. 脉冲安培检测-高效阴离子色谱对药品和保健食品中牛磺酸的快速测定[J].分析测试学报,2009,28(4):470-473.
[8]惠秋沙.薄层扫描法测定保健饮料中牛磺酸的含量[J].食品与药品,2011(7):276-278.
[9]祖如松.食品中牛磺酸的测定方法-薄层层析法[J].中国卫生检验杂志,1998,8(5):292.
[10]孙洁.氨基酸分析仪和HPLC测定食品中牛磺酸的研究比较[J].食品工业,2012,33(8):123-125.
[11]王洪健,周兴起,冯志强,等.氨基酸自动分析仪测定食品中牛磺酸的方法建立[J].现代食品科技,2012,28(3):348-350.
[12]蔡梅,吉文亮,刘华良,等.氨基酸自动分析仪对食品中牛磺酸快速测定方法研究[J].中国卫生检验杂质,2013,23(1):41-45.
[13]张婷,陈雷,刘芸,等.高效液相色谱-高分辨质谱法测定乳粉中的牛磺酸[J].食品安全质量检测学报,2017,8(6):2086-2089.
[14]康明芹,陈明岩,王岸英,等.高效液相色谱-串联质谱法测定保健食品中牛磺酸[J].理化检验(化学分册),2018,54(2):153-155.
[15]邵金良,杨东顺,王丽,等. 固相萃取-高效液相色谱法同时测定牛奶中13种磺胺残留[J].分析实验室,2014,33(11):1322-1325.
[16]朱慧,李克,翟云霞.血清蛋白质组学研究中乙腈沉淀法去除清蛋白的实验研究[J].临床检验杂志,2011(1):16-18.
[17]刘晓云,陈笑艳,钟大放.液相色谱-串联质谱生物分析方法的基质效应和对策[J].质谱学报,2017,38(4):388-399.