固相萃取/^18O标记高氯酸根稀释高效液相色谱-串联质谱法测定水果中的高氯酸盐

Determination of Perchlorate in Fruits by Solid Phase Extraction /^(18)O Labeled Perchlorate Dilution High Performance Liquid Chromatography- Tandem Mass Spectrometry

建立了水果中高氯酸盐的高效液相色谱-串联质谱分析检测方法。样品采用1%乙酸提取,C18固相萃取柱净化,Waters IC-Pak Anion HR(4.6 mm×75 mm)色谱柱洗脱,流动相为乙腈-100 mmol/L乙酸铵溶液(体积比60∶40),流速0.7 m L/min;液相色谱-三重四极杆质谱联用技术-电喷雾负离子监测模式检测,采用18O标记高氯酸根离子作为内标进行基质校正,内标法定量。结果表明:高氯酸盐在0.1~10.0μg/L范围内线性关系良好,定量下限为1.0μg/kg;在1.0,2.0,10μg/kg 3个加标水平下的回收率为92.5%~110%,相对标准偏差(RSD)为1.4%~5.4%。实际样品检测表明该方法准确可靠,适合于水果中高氯酸盐的测定。

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 C18solid-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. An18O-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.