石墨炉原子吸收法测定盐酸伐昔洛韦中钯的残留量.PDFVIP

石墨炉原子吸收法测定盐酸伐昔洛韦中钯的残留量 陈超，俞辉(浙江省食品药品检验所，杭州 310004) 摘要：目的 建立盐酸伐昔洛韦中钯残留量的测定方法。方法 采用微波消解系统消解样品，石墨炉原子吸收分光光度 1 内呈良好线性关系(r=0.999 5) 。检出限为0.20 µg·L1 ， 法测定盐酸伐昔洛韦中钯的残留量。结果 钯在浓度 1.0~30.0 µg·L 定量限为0.95 µg·L1 ，特征浓度(灵敏度)为0.57 µg·L1 ，平均回收率为101.69%。结论 采用本法测定盐酸伐昔洛韦中钯 的残留量灵敏、准确、可靠，为药品质量控制提供依据。 关键词：石墨炉原子吸收分光光度法；钯；盐酸伐昔洛韦 中图分类号：R917.102; R927.12 文献标志码：B 文章编号：1007-7693(2011)03-0260-03 Palladium Residues Determination in Valaciclovir Hydrochloride by Graphite Furnace Atomic Absorption Spectrometry CHEN Chao, YU Hui(Zhejiang Insititute for Food and Drug Control, Hangzhou 310004, China) ABSTRACT: OBJECTIVE To establish a method for the determination of Pd in valaciclovir hydrochloride. METHODS Appling microwave degrading system to deteriorate sample, use a graphite furnace atomic absorption spectrometry (AAS) method to determine Pd residues in valaciclovir hydrochloride. RESULTS It showed a good linear relationship within the concentration range of 1.030.0 µg·L1(r=0.999 5). The LOD and LOQ were 0.20 µg·L1 and 0.95 µg·L1, respectively. The characteristic concentration (sensitivity) was 0.57 µg·L1 and the average recovery was 101.69%. CONCLUSION This method is sensitive, accurate and reliable to control the residues of Pd in valaciclovir hydrochloride, providing the basis for drug quality control. KEY WORDS: graphite furnace atomic absorption spectrometry; palladium; valaciclovir hydrochloride EMEA/CHMP 颁布了金属催化剂或金属试剂 制。钯属于指导文件中第 1 类金属 A 亚组(第 1 类 残留量限度规定的指导文件[1] ，于 2008 年 9 月 1 金属具有显著安全性担忧，共 10 种金属，具有已 日正式实施。在原辅料合成中可能用到金属催化 知的或怀疑的人体致癌性，或者具有其他显著的 剂或金属试剂，这些金属可能在原料药中残留， 毒性；A 亚组包括 2 种金属：P