摘要
考察了药用辅料黄原胶中具有挥发性的汞元素测定方法的稳定性与可靠性。以10 mL硝酸用一定的消解程序进行微波消解,赶酸,加入标准金溶液,稀释,采用电感耦合等离子体质谱法(ICP-MS)测定样品中汞元素的含量,内标法定量。测试结果显示:汞元素的质量浓度在一定范围内与其对应的响应值与内标响应值的比值呈线性关系,检出限为0.0204μg/L;6份加标样品溶液,结果相对标准偏差为11.4%;样品加标回收试验,回收率为87.3%~111.3%。实际样品分析表明,汞元素含量均低于ICH Q3D规定的允许浓度限值。所建立方法专属性好、灵敏度高、准确度强、结果可靠,适用于黄原胶中汞元素的测定。
The stability and reliability of a method for detecting volatile mercury in Xanthan gum are investigated.10 mL of nitric acid was microwave digestion with a certain digestion procedure,rushed acid,added standard gold solution,diluted,and the content of mercury in the sample was determined by ICP-MS,and the internal standard was quantified.The results showed:the mass concentration of mercury element had a linear relationship with the ratio of its corresponding response value to the response value of the internal standard within a certain range.The limit of detection(3.3δ/s)was 0.0204μg/L;6 spiked sample solutions,the relative standard deviation of the result was 11.4%;spiked recovery test of the sample,The accuracy result was 87.3%~111.3%.After analysis of the actual samples,the mercury levels were below the permissible concentration limits specified by ICH Q3D.This established method had good specificity,high sensitivity,strong accuracy and reliable results,and was suitable for the determination of Hg element in xanthan gum.
作者
孙花丽
李利利
张亮亮
张振
侯卫卫
雷洋
门靖
SUN Hua-li;LI Li-li;ZHANG Liang-liang;ZHANG Zhen;HOU Wei-wei;LEI Yang;MEN Jing(Shaanxi Junjing Med Biomedical Technology Co.,Ltd.,Xi’an 712100,China;Xi’an Renalysis Medical Technology Co.,Ltd.,Xi’an 710304,China;Xi’an Wanlong Pharmaceutical Co.,Ltd.,Xi’an 710119,China)
出处
《精细化工中间体》
CAS
2023年第1期92-96,共5页
Fine Chemical Intermediates
