目的: 采用电感耦合等离子体质谱法（IPC-MS 法）及原子荧光光谱法（AFS）测定雪松松针中 28 种 元素的含量。方法: 采用硝酸 - 水体系对雪松松针样品进行微波消解,用原子荧光光谱法测定雪松松针 中的 Hg 元素,Li、Be、Na 等 27 种元素用电感耦合等离子体质谱法进行测定。结果: 28 种元素的线性关 系良好,r ≥ 0.999 2,精密度、重复性、稳定性试验的 RSD 分别小于 4.0%、4.3% 及 3.5%,加样回收率介于 88.6%~110.6% 之间,RSD 均小于 4.9%。15 批雪松松针样品中,K、Mg、Ca、Na、Al、Fe、Sr、Mn、Zn、Ba 元素 的含量较高,参考 2020 年版《中华人民共和国药典》中对于中药材中重金属元素的含量限定,发现 Pb、Cd、 As、Hg、Cu 等重金属及有害元素的含量均未超过限量要求。主成分分析得到 6 个主成分,累计方差贡献率 达 88.68%,确定 Cs、V、Fe、Al、Cr、Se、Co、Tl、Be、As、Ca、K 元素为雪松松针的特征元素。结论: ICP-MS 及 AFS 法测定雪松松针中的 28 种元素,具有准确度高及灵敏性好等特点;本研究对雪松松针的质量控制、深入研究和开发具有一定的潜力和价值。
Objective: To determine 28 kinds of elements in pine needles of Cedrus deodara by inductively coupled plasma mass spectrometry（IPC-MS）and atomic fluorescence spectrometry（AFS）. Methods: These samples were digested by microwave in nitric acid water system,and mercury（Hg）in pine needles was determined by atomic fluorescence spectrometry,and 27 kinds of elements such as Li,Be,Na were determined by inductively coupled plasma mass spectrometry. Results: The linear relationship of 28 elements was good with r ≥ 0.9992. The RSD values of precision,repeatability and stability test were less than 4.0%,4.3% and 3.5% respectively. The recovery rates were between 88.6% and 110.6%,and the RSD values were all less than 4.9%. In 15 batches of samples,the contents of K,Mg,Ca,Na,Al,Fe,Sr,Mn,Zn and Ba were relatively high. Referring to the content limit of heavy metals and harmful elements in traditional Chinese medicine of Pharmacopoeia People’s Republic of China（2020）,it was found that the contents of heavy metal elements such as Pb,Cd,As,Hg and Cu did not exceed the limit. Six principal components were obtained by principal component analysis,and the cumulative variance contribution rate was 88.65%. It was indicated that Cs,V,Fe,Al,Cr,Se,Co,Tl,Be,As,Ca and K were the characteristic elements of the pine needles from Cedrus deodara. Conclusion: The method of ICP-MS and AFS for the determination of 28 elements in pine needles of Cedrus deodara has the characteristics of high accuracy and sensitivity. This study has certain potential and value for the quality control,further research and development of the pine needles from Cedrus deodara.
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