首页|ICP-MS测定不同产地肉苁蓉中多种微量元素的含量

ICP-MS测定不同产地肉苁蓉中多种微量元素的含量

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目的 建立37种元素的微波消解-电感耦合等离子体质谱(ICP-MS)测定方法,并对不同产地的肉苁蓉中37种无机元素进行检测分析,初步探索研究不同产地肉苁蓉中多种无机元素的污染分布情况.方法 以硝酸-过氧化氢为消解试剂,采用微波消解法对样品进行前处理,通过采用在线内标校正,外标法定量ICP-MS法同时测定肉苁蓉中37种无机元素的含量.结果 在曲线范围0.50~100 μg·L-1(Hg:0.20~20μg·L-1)内与峰面积呈良好的线性关系(r≥0.997 4),检出限为0.000 27~0.045μg·L-1,加标回收率在高、中、低3个添加水平下,元素的平均回收率介于76.5%~110.0%,仪器精密度和重复性的相对标准偏差(RSD)值均<4.8%;40批肉苁蓉中5种《中国药典》2020年版明确需要控制的有害重金属元素(铜、铅、砷、汞、镉)的检出率分别为27.5%、7.5%、82.5%、0和100%;钡元素、锰元素、铷元素和锶元素在40批样品检出率均为100%,且含量远远高于其他元素,具有明显的地域性差异.结论 该方法灵敏度高、重现性好、缩短了检验时间、降低了检验成本,可同时检测肉苁蓉中多种无机元素,为肉苁蓉的优化培育和保证药材品质以及用药安全提供数据支撑.
Determination of Trace Elements in Cistanches Herba from Different Habitats by ICP-MS
OBJECTIVE To establish a method for the determination of 37 kinds of inorganic elements by microwave digestion and inductively coupled plasma mass spectrometer(ICP-MS),and to detect and analyze 37 kinds of inorganic elements in cistanches herba from different habitats,and to preliminatively explore the pollution distribution of various inorganic elements in cistanches herba from different habitats.METHODS Using nitric acid and hydrogen peroxide as digestion reagent,microwave digestion was used to pretreat the samples.The contents of 37 inorganic elements in cistanches herba were determined simultaneously by internal standard correction and external standard quantitative ICP-MS method.RESULTS In the curve range of 0.50-100 μg·L-1(Hg:0.20-20 μg·L-1)showed a good linear relationship with the peak area(r≥0.997 4).The detection limits were 0.000 27-0.045μg·L-1.The average recoveries were 76.5%to 110.0%at high,medium and low levels.RSD of precision and repeatability were lower than 4.8%.The detection rates of 5 harmful heavy metal elements(copper,lead,arsenic,mercury,cadmium)that need to be controlled by Chinese Pharmacopoeia(2015 edition)in 40 batches of cistanches herba were 27.5%,7.5%,82.5%,0 and 100%,respectively.The detection rate of barium,manganese,rubidium and strontium in 40 batches of samples is 100%,and the content is much higher than other elements,there are obvious regional differences.CONCLUSION This method has high sensitivity,good reproducibility,reduced the inspection time and cost,and can simultaneously detect various inorganic elements in cistanches herba,providing data support for optimal cultivation,quality assurance and drug safety of cistanches herba.

cistanches herbainorganic elementmicrowave digestionICP-MS

徐勤科、魏学冰、李莉、尉鹏、郭朝晖、孙莺

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甘肃省药品检验研究院,兰州 730000

肉苁蓉 无机元素 微波消解 电感耦合等离子体质谱法

2020年中药材及饮片质量控制重点实验室项目资助

2020GSMPA-KL08

2024

中国药学杂志
中国药学会

中国药学杂志

CSTPCD北大核心
影响因子:0.957
ISSN:1001-2494
年,卷(期):2024.59(2)
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