离子交换色谱-串联质谱法快速测定茶叶中氯酸盐和高氯酸盐OA北大核心CSTPCDMEDLINE

Ion exchange chromatography-tandem mass spectrometry(IEC-MS/MS)has re-cently become the preferred method for detecting ionic substances in tea.In this study,an IEC-MS/MS method was developed for the rapid determination of chlorate and perchlorate residues in tea samples.The optimal sample extraction process,pretreatment column,and chromato-graphic and mass spectrometric conditions were systematically investigated.In the optimal process,the tea samples were ultrasonically extracted with methanol-water(13∶7,v/v),and a PRiME HLB SPE column was used to purify the sample extract.An AceChrom Hybri-A IEC column(150 mm×2.1 mm,5.0 μm)was used for separation,and 100 mmol/L ammonium ace-tate-acetonitrile(40∶60,v/v)was used as the mobile phase for isocratic elution.The flow rate was 0.3 mL/min,the column temperature was 40℃,and the injection volume was 5.0 μL.The mass spectrometric data were collected in negative electrospray ionization mode combined with multiple reaction monitoring(MRM)mode to achieve the rapid and accurate separation and qualitative analysis of the desired chemical components.Quantification was performed using the internal standard(IS)method.The measurement results showed a good linear relationship when the mass concentrations of chlorate and perchlorate were between 2.00-200 and 1.00-100 μg/L,respectively,with correlation coefficients(r2)greater than 0.999 0.The average re-coveries of chlorate and perchlorate at three spiked levels of low,medium,and high ranged from 88.54%to 97.25%with relative standard deviations(RSDs,n=7)of 3.2%-5.2%.The limits of detection for chlorate and perchlorate were 12.0 and 8.0 μg/kg,respectively,while the limits of quantification were 40.0 and 26.6 μg/kg,respectively.The results of tests conduc-ted to assess the linearity,specificity,accuracy,precision,and applicability of the method to the analysis of chlorate and perchlorate in 15 tea samples collected from a local market demon-strated its validity for the routine analysis of tea samples.The proposed method is simple,rap-id,sensitive,and accurate,and can meet requirements for the rapid screening and quantitative analysis of residual trace chlorate and perchlorate in large quantities of tea samples.