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中国医药导刊 ›› 2021, Vol. 23 ›› Issue (4): 281-284.

• 检验检测 • 上一篇    下一篇

微波消解-电感耦合等离子体质谱法测定何首乌药材及黑豆黄酒炮制后饮片中重金属及有害元素含量

 李正刚, 马彧, 刘嘉乐, 赵磊, 赵艳*   

  1. 四平市食品药品检验所, 吉林 四平 136001
  • 收稿日期:2020-11-04 修回日期:2021-03-01 出版日期:2021-04-28 发布日期:2021-04-28
  • 基金资助:
    吉林省地方中药炮制规范项目[项目编号:JLPZGF-2020-014;项目名称:何首乌(黑豆酒炙)]

Determination of Heavy Metals and Harmful Elements in Polygoni Multiflori Radix and Processed Product by Semen Sojae Atricolor and Rice Win  with Miccorowave Digestion-ICP-MS

 LI Zhenggang, MA Yu, LIU Jiale, ZHAO Lei, ZHAO Yan*   

  1. Siping Institute for Food and Drug Control, Jilin Siping 136001, China
  • Received:2020-11-04 Revised:2021-03-01 Online:2021-04-28 Published:2021-04-28

摘要: 目的:建立电感耦合等离子体质谱(ICP-MS)法测定何首乌药材及黑豆黄酒炮制后饮片中铅(Pb)、砷(As)、汞(Hg)、镉(Cd)、铜(Cu)5种重金属及有害元素的含量,为何首乌黑豆酒炙饮片质量控制提供准确、可靠的检测方法及基础数据。方法: 样品经微波消解后,以锗(Ge)、铟(In)、铋(Bi)元素作为内标,进行ICP-MS法测定,射频功率为1.6 kW,采样深度为17.0 mm,载气(高纯氩气)流速为1.1 L·min-1,冷却气流速为15.0 L·min-1,辅助气流量为1.0 L·min-1;扫描次数为20次;重复次数为3次。结果: Pb、As、Cu、Cd、Hg 5种待测元素的线性关系良好(r≥0.997 5),回收率82.18%~108.36%(RSD≤9.59%),方法检测限0.014~0.15 μg·L-1。5批样品炮制前后均不同程度地检出了Pb、As、Cu、Cd 、Hg,测定结果显示炮制前后含量无显著变化。结论: 该方法准确,灵敏度高。何首乌黑豆酒炙的炮制工艺是安全,稳定的。
   

关键词: font-size:medium, ">何首乌;炮制;微波消解;电感耦合等离子体质谱;重金属及有害元素

Abstract: Objective: To establish an inductively coupled plasma mass spectrometry(ICP-MS)method for the determination of the content of 5 kinds of heavy metals and harmful elements [lead(Pb), arsenic (As), mercury (Hg), cadmium (Cd), and copper (Cu)] in Polygoni Multiflori Radix and processed product by semen sojae atricolor and rice wine, to provide accurate and reliable detection methods and basic data for quality control of processed Polygoni Multiflori Radix. Methods: The samples were digested by microwave and calibrated by internal standard elements including Ge,In and Bi, and were analyzed by ICP-MS.The determination conditions were as follows:ICP-MS power was 1.6 kW; the sampling depth was 17.0 mm,the carrier gas (high purity argon) flow rate was 1.1 L·min-1, the cooling gas velocity was 15.0 L·min-1, the auxiliary gas velocity was 1.0 L·min-1, and the sampling was scaned 20 times and repeated 3 times. Results: The 5 kinds of heavy metals and harmful elements showed good linearity within the selected concentration ranges (r≥0.997 5) with the average recovery from 82.18% to 108.36%,while their RSD were below or equal to 9.59%.The detection limits of the method were range from 0.014 to 0.15 μg·L-1. 5 batches of samples before and after processing contained different levels of Pb、As、Hg、Cd and Cu,but no significant change. Conclusion: The method is accurate and sensitive. The processing of Polygoni Multiflori Radix by Semen Sojae Atricolor and rice wine was safe and stable.

Key words: font-size:medium, ">Polygoni Multiflori Radix;Processing; Microwave digestion;Inductively coupled plasma mass spectrometry(ICP-MS); Heavy metals and harmful elements

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