| 孙雨彤,孙震,许雯雯,周凤梅,由春娜,刘万卉.微波消解-ICP-MS法测定罗替戈汀原料药中元素杂质含量[J].中国药事,2021,35(3):289-299 |
| 微波消解-ICP-MS法测定罗替戈汀原料药中元素杂质含量 |
| Determination of Elemental Impurities in Rotigotine by Microwave Digestion ICP-MS |
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| DOI：10.16153/j.1002-7777.2021.03.008 |
| 中文关键词: 罗替戈汀 微波消解 ICP-MS 元素杂质 方法学验证 |
| 英文关键词: Rotigotine microwave digestion ICP-MS elemental impurities method validation |
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| 中文摘要: |
| 目的：建立微波消解电感耦合等离子体质谱法测定罗替戈汀原料药中锂(7 Li)、钒(51V)、 钴(59Co)、镍(60Ni)、铜(65Cu)、砷(75As)、镉(111Cd)、锑(121Sb)、汞(202Hg)、铅 (208Pb)、硼(11B)、钙(44Ca)12种元素杂质含量，对该原料药中元素杂质进行控制。方法：采用微波消解法进行样品前处理，以钪(21Sc)、锗(73Ge)、铽(159Tb)、铋(209Bi)为内标，采用ICP-MS 进行测定，并对建立的方法进行验证。结果：按国际上最新的药典及法规要求对ICP-MS测定元素杂质的分析方法进行了验证：基质干扰＜10%，专属性良好；12种元素在各自的检测浓度范围内r＞0.999； 定量限低于10%限度值；重复性试验RSD均＜6.0%(n=6)；中间精密度试验RSD均＜8%(n=12)；加样回收率为81.0%~114.0%；样品中各元素杂质含量远小于其限度值。结论：研究建立的ICP-MS元素杂质测定方法及评估程序符合目前国际上最新的药典及法规要求，可用于罗替戈汀原料药中元素杂质的质量控制，并为药品质量研究中元素杂质定量分析方法的建立与评估提供参考。 |
| 英文摘要: |
| Objective: To establish a Microwave Digestion-Inductively Coupled Plasma Mass Spectrometry (MD-ICP-MS) method for the determination of 12 kinds of elemental impurities (7 Li, 51V, 59Co, 60Ni, 65Cu, 75As, 111Cd, 121Sb, 202Hg, 208Pb, 11B, 44Ca) in Rotigotine, so as to control the quality of these elemental impurities. Methods: Microwave digestion method was adopted for sample pretreatment, 21Sc, 73Ge, 159Tb, 209Bi were used as internal standard elements, ICP-MS was used for the determination, and the established method was verified. Results: The analytical method for the determination of elemental impurities by ICP-MS was verified according to the latest international pharmacopoeia and regulations. The results showed that the matrix interference was within 10%, indicating that the specificity was good, 12 elements were within the respective detectionconcentration range with the regression coefficients of standard curve beyond 0.999, the limit of quantitation was lower than 10% limit value, the relative standard deviations (RSDs) were within 6.0% (n=6) in the repeatability test, the relative standard deviations (RSDs) were within 8% (n=12) in the intermediate precision test, the recovery rates of spiked samples ranged from 81.0% to 114.0%; the impurity content of each element in the samples was far less than its limit value. Conclusion: The established ICP-MS determination method and the evaluation procedures for elemental impurities conform to the latest international pharmacopoeia and regulatory requirements, which can be used for the quality control of elemental impurities in Rotigotine API, and they will provide references for the establishment and evaluation of quantitative analysis methods for elemental impurities in drug quality researches. |
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