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目的建立高分辨电感耦合等离子质谱(HR-ICP-MS)结合直接稀释血浆样品的前处理,快速测定儿童血浆12种微量元素(B、V、Cr、Mn、Fe、Co、Cu、Zn、Se、Rb、Sr、Mo)。方法血浆样品冻融,4000 r/min离心15 min取上清液,加适量Ga、Y内标溶液,并以0.5%HNO3按1∶20(V/V)直接稀释制备血浆样品,优化调谐HR-ICPMS进行测定。结果仪器检出限0.001~0.035μg/L,方法检出限0.012~0.702μg/L,决定系数(R2)介于0.9983~1.0000,低、中、高加标回收率85.86%~121.34%,方法日内精密度0.52%~5.62%,日间精密度1.21%~10.21%,牛血清质控样品各元素测定值均在100%±15%。应用HR-ICP-MS测定获得了2002年中国居民营养调查贫困农村地区3~12岁儿童血浆12种微量元素基线数据。结论高灵敏度HRICP-MS与0.5%HNO3直接稀释快速制备血浆样品,适合大批量样本多元素快速测定的人群调查。
OBJECTIVE To establish a method for the rapid determination of 12 trace elements (B, V, Cr, Mn, Fe, Co, Cu, Zn, Se) in children by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) combined with direct dilution of plasma samples , Rb, Sr, Mo). Methods Plasma samples were thawed and thawed at 4000 r / min for 15 min. The supernatant was obtained by centrifugation for 15 min. The appropriate amount of Ga and Y internal standard solution was prepared and directly diluted with 0.5% HNO3 at 1:20 (V / V) -ICPMS determination. Results The detection limit was 0.001 ~ 0.035μg / L, the detection limit was 0.012 ~ 0.702μg / L, the determination coefficient (R2) was 0.9983 ~ 1.0000, and the recoveries were 85.86% ~ 121.34% Intra-day precision 0.52% ~ 5.62%, day precision of 1.21% ~ 10.21%, bovine serum quality control sample of the elements were 100% ± 15%. Baseline data of 12 trace elements in plasma of 3 ~ 12-year-old children in impoverished rural areas in China in 2002 were obtained by HR-ICP-MS. Conclusions High sensitivity HRICP-MS and 0.5% HNO3 direct dilution can be used to rapidly prepare plasma samples, which is suitable for the population survey of rapid determination of multi-elements in large samples.