同位素稀释超高效液相色谱-串联质谱法同时测定液态乳中的高氯酸盐和氯酸盐  

Simultaneous Determination of Perchlorate and Chlorate in Liquid Milk by Isotope Dilution Coupled With Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：梁志森 岑建斌 区硕俊 LIANG Zhi-Sen;CEN Jian-Bin;OU Shuo-Jun(Guangzhou Inspection and Testing Certification Group Company,National Quality Testing Center for Processed Food(Guangdong),Guangdong Guangzhou 511447,China)

机构地区：[1]广州检验检测认证集团有限公司国家加工食品质量检验中心(广东)

出　　处：《当代化工》2019年第7期1619-1622,共4页Contemporary Chemical Industry

摘　　要：结合了同位素稀释法和超高效液相色谱-串联质谱法,成功实现对液态乳中的高氯酸盐和氯酸盐的同时测定。样品以水和乙腈提取后,离心分层,上清液用乙酸铵溶液定容。使用同位素内标的质谱响应对结果进行校正。在优化后的色谱及质谱条件下,采用ESI负离子模式进行电离,开通过多反应监测(Multi-selected reaction monitoring,MRM)模式对目标化合物的定量离子和定性离子进行测定。高氯酸盐和氯酸盐在10.0~200μg/L范围内线性良好,相关系数r分别为0.999 7和0.999 6,三个浓度添加水平的平均回收率范围在97.5%~102.0%之间,相对标准偏差为4.32%~5.82%。高氯酸盐和氯酸盐的方法检出限(LOD)为1.5和2.0μg/kg,定量限(LOQ)分别为5.5和8.0μg/kg。该方法操作简便快速,方法学结果表明该方法回收率高、灵敏度高、精密度好,可用于实际测定液态乳中的高氯酸盐和氯酸盐。Simultaneous determination of perchlorate and chlorate in liquid milk was carried out by isotope dilution coupled with ultra performance liquid chromatography-tandem mass spectrometry. After being extracted by water and acetonitrile, the sample was centrifuged. The supernatant was then diluted with ammonium acetate solution. The analytical results were calibrated by MS signals of isotopic internal standard. The sample was determined by a UPLC-MS/MS system operated in a negative electrospray ionization(ESI-) mode under optimized conditions. The quantitative and qualitative ions of target compounds were obtained by multi-selected reaction monitoring(MRM)scanning detection. The calibration curves of perchlorate and chlorate exhibited a good linearity in the range of10.0~200 μg/L, with correlation coefficients of 0.999 7 and 0.999 6, respectively. The average recoveries of three concentration levels ranged from 97.5% to 102.0%. The relative standard deviations(RSDs) were in the range from4.32% to 5.82%. The limits of detection(LOD) of perchlorate and chlorate were 1.5 and 2.0 μg/kg, and the limits of quantitation(LOQ) were 5.5 and 8.0 μg/kg, respectively. This method is efficient to perform, and the methodological results showed that determination of perchlorate and chlorate in liquid milk with this method was practical with high recoveries, good sensitivities, and good precisions.

关 键 词：超高效液相色谱-串联质谱法 液态乳 高氯酸盐和氯酸盐 同位素稀释法 

分 类 号：O0657.63[理学] TQ110.6[化学工程—无机化工]