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    超级微波消解-电感耦合等离子体串联质谱法测定滨海白首乌制品中23种元素及其质量评价

    Determination and Quality Evaluation of 23 Elements in Cynanchum Auriculatum Royle Ex Wight Products Planted in Binhai by Inductively Coupled Plasma Tandem Mass Spectrometry with Super Microwave Digestion

      摘要
    • 摘要: 通过优化消解体系、消解温度、消解时间,采用题示方法测定滨海白首乌制品中Li、Be、V、Cr、Ni、As、Se、Cd、Sn、Sb、Tl、Co、Mo、Al、Mn、Cu、Ba、Zn、K、Ca、Mg、Fe、Na等23种元素的含量。取粉碎后的样品约0.3 g置于石英消解管中,加入1 mL水和2 mL硝酸,混匀后加盖升温至200 ℃并消解10 min,冷却后,用水将消解液稀释至25 mL,采用电感耦合等离子体串联质谱法（ICP-MS/MS）在氦气碰撞模式下测定30份样品中23种元素的含量,并采用SPSS18.0软件对30份样品中均有检出的16种元素进行相关性分析和主成分分析。结果表明,23种元素的质量浓度均在一定范围内和对应的响应强度与内标响应强度之比呈线性关系,检出限（3s）为0.000 3~0.900 mg·kg−1,利用内标法和气体稀释降低基质效应引起的信号漂移；按照标准加入法进行回收试验,回收率为81.2%~115%,测定值的相对标准偏差（n=6）为0.53%~5.0%。样品分析结果表明,滨海白首乌制品中不同元素的含量差异明显,K、Ca、Mg、Na等常量元素含量较高,Mn、Al、Fe、Zn、Ba、Cu含量次之,Li、Be、V、Cr、Ni、As、Se、Cd、Sn、Sb、Tl、Co、Mo含量较低或未检出。相关性分析结果表明,30份滨海白首乌制品中均含有的16种元素之间存在着协同或拮抗的作用。主成分分析结果表明,Ni、Co、Mo、Mn、Cu、Zn、K、Ca、Mg、V、Al、Cr为滨海白首乌制品中的特征元素。

       

      Abstract: By optimizing the digestion system, digestion temperature, and digestion time, the content of 23 elements, including Li, Be, V, Cr, Ni, As, Se, Cd, Sn, Sb, Tl, Co, Mo, Al, Mn, Cu, Ba, Zn, K, Ca, Mg, Fe,and Na in the products of Binhai Cynanchum auriculatum Royle ex Wight was determined using the method shown in the title. About 0.3 g of the crushed sample was taken and placed into a quartz digestion tube, and 1 mL of water and 2 mL of nitric acid were added. The mixture was shaken evenly, sealed and heated up to 200 ℃ to degest for 10 min. After cooling, the digestion solution was diluted to 25 mL with water. Inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) in helium collision mode was used to determine the content of 23 elements in 30 samples, and SPSS18.0 software was used to perform correlation analysis and principal component analysis on the 16 elements detected in all 30 samples. It was shown that linear relationships between the mass concentrations of 23 elements and ratios of corresponding response intensity to internal standard response intensity were kept in definite ranges, with detection limits (3s) in the range of 0.000 3-0.900 mg·kg−1. The signal drift caused by matrix effects was reduced using internal standard method and gas dilution. Test for recovery was made according to the standard addition method, giving recoveries in the range of 81.2%-115%, and RSDs (n=6) of the determined values in the range of 0.53%-5.0%. As found by the sample analysis results, there were significant differences in the content of different elements in the products of Binhai Cynanchum auriculatum Royle ex Wight. The content of constant elements such as K, Ca, Mg and Na was higher, followed by Mn, Al, Fe, Zn, Ba and Cu. The content of Li, Be, V, Cr, Ni, As, Se, Cd, Sn, Sb, Tl, Co and Mo was low or not detected. As found by the correlation analysis results, there was a synergistic or antagonistic effect between the 16 elements contained in all 30 products of Binhai Cynanchum auriculatum Royle ex Wight. As found by the principal component analysis results, Ni, Co, Mo, Mn, Cu, Zn, K, Ca, Mg, V, Al and Cr were characteristic elements in the products of Binhai Cynanchum auriculatum Royle ex Wight.

       

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