超级微波消解电感耦合等离子体发射光谱法同时测定禹余粮药材中9种元素含量  

Simultaneous Determination of Nine Elements in Limonitum by Super Microwave Digestion Combined with ICP-OES

作　　者：冷崇姣 刘清士 揭定华 赵贵琴 侯小梅 LENG Chongjiao;LIU Qingshi;JIE Dinghua;ZHAO Guiqin;HOU Xiaomei(Yongchuan District Institute for Food and Drug Control,Chongqing,China 402160;Hangzhou Puyu Technology Co.,Ltd.,Hangzhou,Zhejiang,China 311300)

机构地区：[1]重庆市永川食品药品检验所,重庆402160 [2]杭州谱育科技发展有限公司,浙江杭州311300

出　　处：《中国药业》2023年第8期65-69,共5页China Pharmaceuticals

基　　金：重庆市永川区自然科学基金[2022yc-lhzz10003]。

摘　　要：目的建立同时测定禹余粮药材中9种元素含量的超级微波消解电感耦合等离子体发射光谱(ICP-OES)法。方法优选的消解程序为50 mg药材粉末样品中加入超纯水1 mL、硝酸0.5 mL、盐酸1.5 mL及氢氟酸2 mL,在240℃、3.5 MPa条件下消解30 min。ICP-OES仪射频功率1150 W,雾化气流量0.7 L/min,冷却气流量12 L/min,辅助气流量1.0 L/min,轴向观测,分析泵速30 r/min,PFA同心雾化器,PFA旋流雾化室,重复3次,检测波长分别为396 nm(铝)、259 nm(铁)、257 nm(锰)、251 nm(硅)、193 nm(砷)、220 nm(铅)、194 nm(汞)、214 nm(镉)、327 nm(铜)。结果铝、铁、锰、硅质量浓度在0~20μg/mL,砷、铅、汞、铜质量浓度在0~10μg/mL,镉质量浓度在0~4μg/mL范围内与信号强度线性关系良好;各元素的检测限为0.1~13.8μg/L;精密度试验结果的RSD为1.02%~3.85%(n=6),砷、汞、镉未检出;平均提取回收率为96.28%~103.92%,RSD为0.91%~4.98%(n=6)。结论所建方法可用于测定禹余粮药材中9种元素含量,结果准确,且简单、高效、环保。Objective To establish a super microwave digestion combined with inductively coupled plasma-optical emission spectrometry(ICP-OES)method for the simultaneous determination of nine elements in limonitum.Methods The optimal digestion procedure was as follows:adding 1 mL of ultra-pure water,0.5 mL of nitric acid,1.5 mL of hydrochloric acid,and 2 mL of hydrofluoric acid to a 50 mg limonitum powder sample,and digesting for 30 min at 240℃and 3.5 MPa.The RF power of the ICP-OES instrument was 1150 W,the flow rate of atomization gas was 0.7 L/min,the flow rate of cooling gas was 12 L/min,and the flow rate of auxiliary gas was 1.0 L/min.Axial observation was performed,the analysis pump speed was 30 r/min,the PFA concentric atomizer and the PFA swirling atomization chamber were adopted for three times,the detection wavelength was set at 396 nm(aluminum),259 nm(iron),257 nm(manganese),251 nm(silicon),193 nm(arsenic),220 nm(lead),194 nm(mercury),214 nm(cadmium),and 327 nm(copper),respectively.Results The linear range of aluminum,iron,manganese,and silicon was 0-20μg/mL,the linear range of arsenic,lead,mercury,and copper was 0-10μg/mL,and the linear range of cadmium was 0-4μg/mL.The limit of detection(LOD)of each element was in the range of 0.1-13.8μg/L.The RSD of the precision tests was in the range of 1.02%-3.85%(n=6),and arsenic,mercury,and cadmium were not detected.The average recovery rate of each element was in the range of 96.28%-103.92%,and the RSD was in the range of 0.91%-4.98%(n=6).Conclusion The established method is accurate,simple,efficient,and environmentally friendly,which can be used to determine the content of nine elements in limonitum.

关 键 词：矿物药 禹余粮 重金属元素 超级微波消解 电感耦合等离子体发射光谱法 含量测定 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]