超高效液相色谱-串联质谱法测定液态乳中的19种全氟烷基化合物  

Determination of 19 fluorinated alkyl compounds in liquid milk by ultra-high performance liquid chromatography-tandem mass spectrometry

作　　者：孙晨 王溪 杨润[1] SUN Chen;WANG Xi;YANG Run(Jiangsu Provincial Center for Disease Control and Prevention,Jiangsu Nanjing 210009,China)

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009

出　　处：《中国食品卫生杂志》2024年第12期1325-1332,共8页Chinese Journal of Food Hygiene

摘　　要：目的建立通过HLB-P/HMR-Lipid SPE净化柱前处理,超高效液相色谱-串联质谱同时检测液态乳中19种全氟烷基化合物的方法。方法样品经乙腈溶解,沉淀蛋白,涡旋提取,使用商品化的双层固相萃取柱HLB-P/HMR-Lipid SPE进行除脂净化,氮吹后甲醇-水(8+2)复溶,以甲醇和2 mmol/L甲酸铵溶液作为流动相梯度洗脱,目标物经ACQUITY Premier BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)分离,使用电喷雾离子源、负离子多反应监测模式进行检测,内标法定量。结果19种全氟烷基化合物在0.1~50μg/L范围内线性关系良好,相关系数r均>0.995。检出限在0.0037~0.0095μg/kg,定量限在0.0124~0.0317μg/kg。液态乳中低浓度加标0.1μg/kg、中浓度加标1μg/kg、高浓度加标8μg/kg,3个添加浓度水平的加标回收率为73.8%~113.1%,相对标准偏差均<10%(n=6)。结论该方法准确可靠、灵敏度高、重现性好,覆盖的全氟化合物种类多,适用于液态乳中全氟烷基化合物的检测。Objective To optimize the sample pretreatment process by using HLB-P/HMR-Lipid SPE purification column.In combination with ultra-high performance liquid chromatoplc-tandem mass spectrometry,a method for simultaneous detection of 19 fluorinated alkyl compounds in liquid milk was established.Methods The sample was extracted by means of acetonitrile dissolving precipitated protein vortex,and the commercial double-layer solid phase extraction column HLB-P/HMR-Lipid SPE was used to purify the lipid.Then the methanol-water(8∶2,v/v)was redissolved after nitrogen blowing,and the mobile phase gradient elution was performed by using methanol and 2mmol/L ammonium formate solution.The targets were separated by ACQUITY Premier BEH C_(18)column(100 mm×2.1 mm,1.7μm),detected by electrospray ion source and negative ion multi-reaction monitoring mode,and quantified by internal standard method.Results The linear relationships of 19 fluorinated alkyl compounds were good in the range of 0.1-50μg/L,and the correlation coefficient r was greater than 0.995.The limit of detection was 0.0037-0.0095μg/kg and the limit of quantification was 0.0124-0.0317μg/kg.The recoveries of low concentrations(0.1μg/kg),medium concentrations(1μg/kg)and high concentrations(8μg/kg)in liquid milk ranged from 73.8%to 113.1%,the relative standard deviations were less than 10%(n=6).Conclusion The method is accurate,reliable,sensitive,reproducible and suitable for the detection of fluorinated alkyl compounds in liquid milk.

关 键 词：超高效液相色谱-串联质谱 液态乳 全氟烷基化合物 

分 类 号：R155[医药卫生—营养与食品卫生学]