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机构地区:[1]黄河科技学院纳米研究所,郑州450063 [2]濮阳市天元虫草研究有限公司,河南濮阳457000
出 处:《中国药房》2017年第12期1684-1686,共3页China Pharmacy
基 金:河南省产学研项目(No.162107000038);河南省高等学校重点科研项目(No.17B360005)
摘 要:目的:建立同时测定人工蛹虫草中4种重金属元素含量的方法。方法:采用硝酸加热法消解样品,采用电感耦合等离子体质谱法进行测定:射频功率为1.15 k W,采样深度为65 mm,辅助气流速为1.0 L/min,冷却气体流量为13.0 L/min,环境温度为25℃,自动等离子体观测。结果:砷、镉、汞、铅检测质量浓度线性范围分别为0~20μg/m L(r=0.997 0)、0~10μg/m L(r=0.999 5)、0~5μg/m L(r=0.995 5)、0~20μg/m L(r=0.996 0);检测限分别为0.128、0.003、0.002、0.004 mg;精密度、稳定性、重复性试验的RSD<6.5%;加样回收率分别为90.4%~100.6%(RSD=3.45%,n=9)、94.3%~101.3%(RSD=2.93%,n=9)、90.0%~102.3%(RSD=4.03%,n=9)、92.3%~103.0%(RSD=3.53%,n=9)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于人工蛹虫草中4种重金属元素含量的同时测定;所测10批人工蛹虫草中As、Cd、Hg、Pb 4种重金属元素含量均符合国家相关标准。OBJECTIVE: To establish the method for the simultaneous determination of contents of 4 heavy metal elements in cultured Cordyceps militaris. METHODS: The samples were digested by nitric acid heating method and then determined by ICP-MS including radio-frequency power of 1.15 kW, sampling depth of 65 nm, auxiliary gas flow rate of 1.0 L/rain, cooling gas flow of 13.0 L/min, temperature of 25 ℃, automatic plasma. RESULTS: The linear ranges of arsenic (As) ,cadmium (Cd), mercury (Hg) and lead (Pb) were 0-20 gg/mL(r=0.997 0), 0-10 gg/mL(r=0.999 5), 0-5 gg/mL(r=0.995 5), 0-20 btg/mL(r= 0.996 0), respectively. Detectio limit were 0.128,0.003,0.002,0.004 mg. RSDs of precision, stability and reproducibility tests were all lower than 6.5%. Recoveries of them were 90.4% -100.6% (RSD=3.45% , n=9) , 94.3% -101.3% (RSD=2.93% , n=9), 90.0%-102.3% (RSD=4.03%, n=9), 92.3%-103.0% (RSD=3.53%, n=9), respectively. CONCLUSIONS : The method is simple, precise, stable, reproducible, and can be used for simultaneous determination of contents of 4 heavy metal elements in cultured C. militaris. The contents of As, Cd, Hg and Pb in 10 batches of sample are all in line with related national standards.
关 键 词:人工蛹虫草 重金属 电感耦合等离子体质谱
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