微波消解-ICP-MS分析不同破壁方法灵芝孢子粉中无机元素含量

Determination of Inorganic Elements in Ganoderma Lucidum Ganoderma Lucidum Spore Powder with Different Treatments of Wall-broken Methods by Microwave Digestion-ICP-MS

关键词:  灵芝孢子粉  破壁方法  电感耦合等离子体质谱  无机元素

Key words:  Ganoderma Lucidum spore powder  wall-broken methods  ICP-MS  inorganic elements

摘要:

目的 建立电感耦合等离子体质谱(ICP-MS)测定灵芝孢子粉中无机元素的方法，比较不同破壁方法灵芝孢子粉中V、Cr、Mn、Fe、Co、Ni、Cu、Zn、Pb、As、Se、Cd、Sn、Sb、Ti、Hg16种元素的含量。方法 微波消解处理灵芝孢子粉，采用ICP-MS同时测定样品中16种元素的含量。结果 16种元素方法检出限为0.000 2~0.101 5 μg·L^-1，线性关系良好( r >0.999 0)，平均回收率为80%~120%，RSD均<5%。与原料相比，破壁后样品中Cr、Fe、Ni、Co等元素含量显著升高( P <0.05或 P <0.01)，但超音速气流破壁样品升高倍数比振动磨破壁样品低1.75~48倍。结论 本方法灵敏度高、快速准确，可用于灵芝孢子粉中无机元素的测定。超音速气流法不易引入重金属污染，是一种安全可靠的破壁工艺。

Abstract:

OBJECTIVE To establish an ICP-MS method to determine the inorganic elements including V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pb, As, Se, Cd, Sn, Sb, Ti and Hg in Ganoderma Lucidum spore powder, and to compare the effects of two different wall-broken methods on the contents of above 16 elements. METHODS Microwave digestion coupled with ICP-MS were carried out to experiment on simultaneous determination of 16 inorganic elements in spore powder. RESULTS The validated method indicated that correlative coefficients( r ) for all elements were >0.999 0, and the limits of detection ranged from 0.000 2-0.101 5 μg·L^-1. The average spiked recoveries were 80%?120% with the RSD<5%. Compared with the crude spore powder, the contents of Cr, Fe, Ni, Co increased remarkably after treated with wall-broken methods ( P <0.05 or P <0.01). However, the multiples of supersonic stream samples were 1.75-48 times smaller than those of vibration mill ones. CONCLUSION The established method is proved to be accurate, rapid and sensitive. Moreover, supersonic stream method reduces heavy metal contamination during wall breaking, which can be further developed as a safe and reliable wall-broken method for spore powder.