ICP-MS法测定无载体三氯化镥[177Lu]溶液中的元素杂质

Determination of elemental impurities in carrier-free lutetium chloride [177Lu] solution by ICP-MS

关键词:  无载体三氯化镥[₁₇₇^Lu]溶液  元素杂质  ICP-MS  ICH Q3D(R2)

Key words:  carrier-free lutetium chloride [_¹77^{Lu] solution}  elemental impurities  ICP-MS  ICH Q3D(R2)

摘要:

目的 建立电感耦合等离子质谱法(ICP-MS)测定国产无载体三氯化镥[₁₇₇^Lu]溶液中的元素杂质的方法。方法 以Sc、Y、In、Bi为内标,采用ICP-MS方法测定,射频功率为1550 w,载气流量0.8 L . min^_-1,蠕动泵转速40 rpm,雾化室温度2.7℃,采样深度5 mm,分析模式为KED。并对所建立的方法进行方法学验证。结果 各元素在线性范围内线性关系良好(r均大于0.9990),低、中、高三个浓度加样回收率(n=9)均在81%~109%之间。测定3批国产无载体三氯化镥[₁₇₇^Lu]溶液样品,结果3批样品中ICH Q3D(R2)元素指导原则中1类、2A类和2B类元素杂质均未检出或远低于注射用PDE。结论 该方法灵敏度、精密度、准确度良好,适用于无载体三氯化镥[₁₇₇^Lu]溶液元素杂质的质量控制。

Abstract:

OBJECTIVE To establish an inductively coupled plasma-mass spectrometry (ICP-MS) method for determining elemental impurities in domestically produced carrier-free lutetium chloride [177Lu] solution. METHODS With Sc, Y, In, and Bi Used as internal standards, an ICP-MS methord was developed and established with the following conditions: RF power of 1550 W, carrier gas flow rate of 0.8 L?min-1, peristaltic pump speed of 40 r?min-1, nebulization chamber temperature of 2.7°C, sampling depth of 5 mm. The method was validated for key analytical parameters. RESULTS Each elements exhibited good linearity within the specified ranges (r > 0.9990), the recovery rates at low, medium and high concentrations were 81% - 109%. Three batches of carrier-free lutetium chloride [177Lu] solution samples were tested, the test results indicated that Class 1, Class 2A, and Class 2B elemental impurities specified in the ICH Q3D(R2) guidelines were either not detected or well below the PDE for injection products. CONCLUSION The developed method demonstrates high sensitivity, good precision, and accuracy, making it suitable for quality control of elemental impurities in carrier-free lutetium chloride [177Lu] solution.