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| Determination of Perchlorate in Fruits by Solid Phase Extraction/18O Labeled Perchlorate Dilution High Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:perchlorate 18O-labelled perchlorate dilution solid phase extraction high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) fruits |
| Author | Institution |
| WU Ying-xuan*,LIN Feng,YAO Yang-xun,SHAO Lin-zhi,OUYANG Shao-lun |
1.广东出入境检验检疫局检验检疫技术中心;2.广东省动植物与食品进出口技术措施研究重点实验室 |
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| Abstract: |
| An analytical method based on high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was developed for the determination of perchlorate in fruits.Samples were extracted with 1% acetic acid.The extract was cleaned up on an C18 solid-phase extraction(SPE) cartridge,and separated on a Waters IC-Pak Anion HR column(4.6 mm×75 mm) using acetonitrile -100 mmol/L ammonium acetate(60∶40) as mobile phase at a rate of 0.7 mL/min.The detection of perchlorate anion was performed by high performance liquid chromatography triple stage quadrupole mass spectrometry,equipped with electrospray ionization(ESI) in the negative ion mode.An 18O labelled perchlorate anion internal standard was used to correct matrix effects.Quantification analysis was conducted by the internal standard calibration.Good linearity was observed for perchlorate in the concentration range of 0.1- 10.0 μg/L.The limit of quantitation was 1.0 μg/kg.The recoveries of perchlorate in different samples at three spiked levels of 1.0,2.0,10.0 μg/kg were in the range of 92.5%-110%,with relative standard deviations of 1.4%-5.4%.The real sample analysis showed that this method was accurate and could be applied in the determination of perchlorate in fruits. |
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