高效液相色谱-串联质谱法测定乳制品中高氯酸盐  

Determination of perchlorate in dairy products by high performance liquid chromatography-tandem mass spectrometry

作　　者：吴映璇[1,2] 林峰[1,2] 谢敏玲 姚仰勋[1,2] 蓝草[1,2] 陈思敏[1,2] WU Ying-xuan LIN Feng XIE Min-ling YAO Yang-xun LAN Cao CHEN Si-min(Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangdong Guangzhou 510623, China 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)

机构地区：[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

出　　处：《中国食品卫生杂志》2017年第2期160-164,共5页Chinese Journal of Food Hygiene

基　　金：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)

摘　　要：目的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,6μm)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0.1~10.0μg/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3.0μg/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。Objective 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 chromatographytandem 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 to10.0 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.

关 键 词：高氯酸盐 固相萃取 同位素 高效液相色谱-串联质谱 乳制品 测定 

分 类 号：O657.63[理学—分析化学] TS252.7[理学—化学]