高效液相色谱-串联质谱法测定乳制品中高氯酸盐
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(1.广东出入境检验检疫局检验检疫技术中心,广东 广州 510623;2.广州出入境检验检疫局 广东省动植物与食品进出口技术措施研究重点实验室,广东 广州 510623)

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吴映璇 女 高级工程师 研究方向为食品安全检测E-mail:allanwyx@126.com

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基金项目:

广东省科技计划项目(2014A040401064);广东检验检疫局科技计划项目(2015GDK10);检验检疫行业标准计划项目(2009B535);国家质检总局项目(2012IK150)


Determination of perchlorate in dairy products by high performance liquid chromatography-tandem mass spectrometry
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(1.Guangdong Entry-Exit Inspection and Quarantine Bureau,Guangdong Guangzhou 510623,China;2.Key Laboratory of Animals and Plants and Food Import and Export of Technical Measures in Guangdong Province, Guangdong Entry-Exit Inspection and Quarantine Bureau,Guangdong Guangzhou 510623,China)

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    摘要:

    建立乳制品中高氯酸盐的高效液相色谱-串联质谱定量分析检测方法。方法 样品采用1%乙酸-乙腈溶液(1∶2,V/V)提取,C18固相萃取柱净化,在IC-PakTM Anion HR色谱柱(4.6 mm×75 mm,6 μm)上,以乙腈-乙酸铵溶液(60∶40,V/V)作为流动相,等度分离。采用液相色谱-质谱联用技术-电喷雾离子源多反应监测模式检测,内标法定量。结果 高氯酸盐在0.1~10.0 μg/L范围内具有良好的线性关系,牛奶和奶粉的定量限分别为1.0和3.0 μg/kg;在三个添加水平下回收率范围在87.6%~122.0%之间,相对标准偏差(RSD)范围为2.0%~10.0%。结论 本方法灵敏、准确,适用于乳制品中高氯酸盐的分析测定,具有较好的实际应用价值。

    Abstract:

    An analytical method based on high performance liquid chromatography-tandem mass spectrometry was developed for the determination of perchlorate in dairy products.Methods Samples were extracted with 1% acetic acide-acetonitrile solution(1∶2,V/V), and the extract was then cleaned up on an solid-phase extraction(SPE)cartridge and separated on a IC-PakTM Anion HR column(4.6 mm×75 mm,6 μm) by using acetonitrile and ammonium acetate solution(60∶40, V/V) as mobile phase. The analytes were determined by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with electrospray ionization source in multiple reaction monitoring(MRM). The internal standard calibration was used for quantification. Results Good linearity was observed in the range of 0.1 to 10.0 μg/L. The limit of quantitation of the established method was 1.0 μg/kg in milk and 3.0 μg/kg in milkpowder. The recovery rate of perchlorate was 87.6%-122.0% at three spiked levels in deferent samples, with relative standard deviation of 2.0%-10.0%.Conclusion The method was sensitive, accurate, and suitable for the analysis of perchlorate in dairy products.

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吴映璇,林峰,谢敏玲,姚仰勋,蓝草,陈思敏.高效液相色谱-串联质谱法测定乳制品中高氯酸盐[J].中国食品卫生杂志,2017,29(2):160-164.

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  • 收稿日期:2016-12-14
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  • 在线发布日期: 2017-05-03
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