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作 者:李智明 邓鸣 朱健萍 李务荣 孙煜 徐光辉 王健 LI Zhiming;DENG Ming;ZHU Jianping;LI Wurong;SUN Yu;XU Guanghui;WANG Jian(Guangxi Institute for Drug Control,Nanning 530021,China;COFCO Chongzuo Sugar Company Limited,Guangxi Sugarcane Industry Chain Extension Engineering Research Center,Chongzuo 532200,China;COFCO Nutrition&Health Research Institute Limited,Beijing Key Laboratory of Nutrition,Health and Food Safety,Beijing 102209,China)
机构地区:[1]广西壮族自治区药品检验研究院,南宁530021 [2]中粮崇左糖业有限公司,广西甘蔗产业链延伸工程研究中心,广西崇左532200 [3]中粮营养健康研究院有限公司,营养健康与食品安全北京市重点实验室,北京102209
出 处:《化学分析计量》2024年第12期82-88,共7页Chemical Analysis And Meterage
摘 要:建立电感耦合等离子体质谱(ICP-MS)法半定量扫描、全定量测定药用辅料蔗糖中元素。采用硝酸作为消解液,经微波消解处理样品后,用ICP-MS半定量进行全谱图快速扫描,筛查出Ti、Cr、Mn、Rb、Sr、Ba、Fe7种元素;再用ICP-MS全定量对所筛查出的元素进行测定。Fe的质量浓度在5~50 ng/mL、其余6种元素质量浓度在1~20 ng/mL范围内存在良好的线性关系,相关系数均大于0.999,检出限为0.001~0.01 mg/kg。样品加标回收率为92.8%~98.9%,测定结果的相对标准偏差为1.5%~2.5%(n=6)。半定量分析能快速筛查样品中所含元素,全定量测定可同时测定多种元素,该方法适用于药用辅料蔗糖中元素的测定。A method was developed to determine seven elements in sucrose as pharmaceutical excipient by inductively coupled plasma mass spectrometry(ICP-MS)semi-quantitative scanning and full quantitative determination.The sample was subjected to microwave digestion with nitric acid,full spectrum was quickly scanned out seven elements including Ti,Cr,Mn,Rb,Sr,Ba,Fe by ICP-MS semi-quantitative scanning.ICP-MS full quantitative determination was used to determine the screened elements.The linear was good for 7 elements within the range of concentration of 1-20 ng/mL except Fe(5-50 ng/mL),the correlation coefficients were all more than 0.999,the detection limits were 0.001-0.01 mg/kg.The recovery rates of sample spiked were 92.8%-98.9%,and the relative standard deviations of the measurement results were 1.5%-2.5%(n=6).The semi-quantitative analysis could quickly screen element contained in the samples,and full quantitative determination could simultaneously measure multiple elements.The method is suitable for determination of elements in sucrose as pharmaceutical excipient.
关 键 词:电感耦合等离子体质谱法 半定量 全定量 药用辅料蔗糖 元素
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