微波消解-ICP-MS法测定不同炮制工艺、产地鲜竹沥中20种微量元素

Determination of 20 trace elements in Fresh Bamboo Juice with different origins and processing methods by microwave digestion-ICP-MS

目的建立微波消解-ICP-MS法测定鲜竹沥中20种元素的测定方法,并考察不同产地和炮制工艺间的区别。方法微波消解样品后,采用ICP-MS,射频功率为1510W,采样深度为7.6mm,载气流速为0.8L·min^(-1),辅助气流速为0.35L·min^(-1),泵速为0.10r·s^(-1),离子透镜1∶3.5V,离子透镜2:-99.5V,反应模式为He模式,He流速为4.5mL·min^(-1)。结果20种元素线性方程的相关系数为0.9992~0.9999,加标回收率为95.3%~107.6%,所有元素的检出限在0.06~10.2ng·mL^(-1)之间,精密度、重复性、稳定性良好。结论鲜竹沥中Mg、K、Ca、Mn、Fe、Zn含量最高,传统直火烧制工艺的鲜竹沥中Mg、K、Ca、Mn、Fe、Zn的含量均普遍高于现代干馏工艺,传统直火烧制工艺下产地为江西3个地域普遍均高于湖南怀化。传统直火烧制工艺Pb、As、Cr均有检出,而现代干馏工艺仅检出Cr,结合每日摄入量分析,Pb、As元素按照每日最大摄入量均高于PDE值,存在摄入风险。

OBJECTIVE To establish ICP-MS method for determine the contents of 20 elements in Fresh Bamboo Juice,and investigate differences between different origins and processing methods.METHODS After microwave digestion of samples,20 elements were determined by ICP-MS.RF power is 1510W,sampling depth is 7.6mm,carrier gas flow rate is 0.8L·min^(-1),auxiliary gas flow rate is 0.35L·min^(-1),pump speed is 0.10r·s^(-1),ion lens 1∶3.5V,ion lens 2:-99.5V.The reaction mode was helium mode with a helium flow rate of 4.5mL·min^(-1).RESULTS The correlation coefficients of the linear equations for 20 elements were 0.9992~0.9999,the recoveries were 95.3%~107.6%,the detection limits of all elements were between 0.06 and 10.2ng·mL^(-1),the precision,repeatability and stability were higher.CONCLUSION The contents of Mg,K,Ca,Mn,Fe and Zn in Fresh Bamboo Juice were the highest.The contents of Mg,K,Ca,Mn,Fe and Zn in Fresh Bamboo Juice by traditional direct firing process were generally higher than that in modern dry distillation process,and those in Jiangxi Province were generally higher than those in Huaihua,Hunan Province.Pb,As and Cr were detected in traditional direct firing process,while Cr was detected in modern dry distillation process only.Combined with daily intake analysis,Pb and As elements were higher than PDE according to the daily maximum intake,indicating a risk of ingestion.