离子交换高效液相色谱-串联质谱法测定鸡肉和鸡肝中的高氯酸盐

Determination of Perchlorate in Chicken Meat and Liver by Ion Exchange High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立测定鸡肉和鸡肝中高氯酸盐的离子交换高效液相色谱-串联质谱法。试样加^(18)O标记高氯酸根离子后采用1%乙酸溶液-乙腈提取,固相萃取柱净化后,经IC-Pak^(TM)Anion HR(4.6 mm×75 mm,6μm)色谱柱分离,以乙腈-100 mmol/L乙酸铵溶液为流动相,采用电喷雾离子源串联质谱,在负离子扫描方式下以多反应监测模式检测,内标法定量。结果表明:高氯酸盐在0.2~10μg/L质量浓度范围内线性关系良好,定量限为3.0μg/kg。在3个加标水平下的平均回收率为91.8%~96.0%,相对标准偏差为1.8%~6.5%。该方法操作简便、灵敏度高、抗干扰能力强、回收率和重复性良好,适用于鸡肉和鸡肝中高氯酸盐的测定。

A method was developed for the determination of perchlorate in chicken meat and liver by ion- exchange highperformance liquid chromatography-tandem mass spectrometry （IC-HPLC-MS/MS）. After adding isotopically labeledinternal standards to it, the sample was extracted with 1% acetic acid-acetonitrile, and then purified by solid-phase extractioncolumn. The target compound was separated on an IC-PakTM Anion HR column （4.6 mm × 75 mm, 6 μm） using a mobilephase consisting of acetonitrile and 100 mmol/L aqueous ammonium acetate, and detected by tandem mass spectrometryin negative electrospray ionization and multiple reaction monitoring （MRM） mode. The quantification of perchlorate wasperformed by the internal standard method. The calibration curves showed good linearity in the concentration range of0.2–10 μg/L with a limit of quantification （LOQ） of 3.0 μg/kg. The recoveries in chicken meat and liver at three spiked levelswere in the range of 91.8%–96.0% with relative standard deviations （RSDs） between 1.8% and 6.5%. With the advantagesof convenience, high sensitivity, strong anti-interference capability and good recovery and repeatability, the method wassuitable for the analysis of perchlorate in chicken meat and liver.