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电感耦合等离子体发射光谱-内标法测定白茶中水溶性硅的含量

Inductively Coupled Plasma Atomic Emission Spectrometry with Internal Standards for Water-Soluble Silicon Determination in White Tea

  • 摘要:
    目的 建立以电感耦合等离子体发射光谱-内标法测定白茶中水溶性硅含量的方法,为研究白茶中的水溶性硅提供科学可靠的检测手段。
    方法 白茶样品经粉碎、过5.0 μm 标准筛,80℃烘干处理后,首先进行不同内标元素(铱、铟、锗)与硅的不同分析谱线的选择实验,并对称样量(1.00、2.00、3.00、4.00、5.00、6.00 g)、沸水浴浸提时间(20、40、60、90、120 min)等样品前处理条件进行优化。确定实验条件后,样品经沸水浴浸提、过滤、加入内标元素、定容,再采用电感耦合等离子体发射光谱法建立测定茶叶中水溶性硅含量的方法,并从精密度、回收率等方面进行方法学考察及白茶样品的测定应用。
    结果 选取内标元素铱(分析谱线224.268 nm)与硅(分析谱线288.158 nm)时,检测结果的精密度及回收率最优。样品前处理最佳实验条件为称样量4.00 g、沸水浴浸提时间90 min。建立的电感耦合等离子体发射光谱-内标法的标准曲线线性良好,相关系数大于0.9999,方法检出限为7.5 µg·L−1,精密度相对标准偏差(RSD)为1.53%,样品加标回收率为99.4%~104.8%。检测采集到的10个白茶样品,其中白牡丹、寿眉各4个(存储时间分别为1、3、7、10年),白牡丹(抛荒茶)2个(存储时间分别为1、3年),结果显示寿眉随着存储年份的增加水溶性硅的含量呈现增长趋势,而不同年份的白牡丹却保持相对稳定,白牡丹(抛荒茶)水溶性硅的含量明显低于其他品类。
    结论 该方法精密度好、检测结果可靠,适用于白茶中水溶性硅含量的测定。不同白茶品类的水溶性硅含量有明显区别,深入研究白茶中的水溶性硅,为探寻白茶的保健功效及品质提升提供新的思路。

     

    Abstract:
    Objective A method for determining the content of water-soluble silicon in white teas using inductively coupled plasma atomic emission spectrometry (ICP-AES) with internal standards was developed.
    Method The ICP-AES procedures were first optimized using the internal standards of iridium, indium, germanium, and silicon with 1.00, 2.00, 3.00, 4.00, 5.00, and 6.00 g sample weights in a boiling water bath for a 20, 40, 60, 90, or 120 m extraction. White tea samples were ground, filtered through a 5.0 μm sieve, and oven-dried at 80oC for more than 4 h as a pretreatment prior to spiking the filtrate with the internal standards and making up to volume. Water-soluble silicon was determined by the optimized ICP-AES, and the results correlated to the standard curve.
    Result The linearity of the silicon measurement curve against iridium standard showed the highest correlation coefficient of greater than 0.9999 with a detection limit of 7.5 µg·L−1, a relative standard deviation (RSD) of 1.53%, and a recovery rate on spiked standards of 99.4%-104.8%. On the 10 white tea specimens, including 4 Baimudan and 4 Shoumei stored for one, 3, 7, and 10 years, and 2 Paohuang Baimudan (Baimudan tea made of leaves from bushes not plucked for years) stored for one and 3 years, the content of water-soluble silicon in Shoumei increased with increasing storage age, while Baimudan of different ages remained relatively constant; and that in Paohuang Baimudan was significantly lower than those in the others.
    Conclusion The newly developed ICP-AES assay was precise and reliable in detecting water-soluble silicon in white teas. It was considered adequate for the determination. By unveiling the differences in the content, in-depth studies on the health effect of varied white teas and quality improvement for new products were significantly facilitaed.

     

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