机构地区:[1]中国人民解放军联勤保障部队第九〇〇医院,福建福州350025
出 处:《中国药业》2025年第7期85-89,共5页China Pharmaceuticals
摘 要:目的建立同时测定连钱草中钾(K)、钙(Ca)、钠(Na)、镁(Mg)、铝(Al)、锌(Zn)、铁(Fe)、锰(Mn)、硒(Se)、镉(Cd)、铅(Pb)、铜(Cu)、硼(B)、铬(Cr)、钡(Ba)、汞(Hg)、钼(Mo)、钴(Co)、砷(As)19种无机元素含量的电感耦合等离子体质谱(ICP-MS)法,确定无机元素分布特征的化学计量学分析方法。方法采用微波消解法对样品进行前处理,等离子体氩气流量为17 L/min,载气流量为1.5 L/min,采样深度为11 mm,雾化室温度为3.0℃,测量模式为碰撞池动能歧视(KED)模式,碰撞气流量为6.5 mL/min,进样冲洗时间为45 s,蠕动泵泵速为60 r/min,以钪(45Sc)、铟(115In)、铋(209Bi)为内标,建立无机元素特征图谱,并采用主成分分析(PCA)及正交偏最小二乘法判别分析(OPLS-DA)评价其特征元素。结果19种无机元素在各自质量浓度范围内与待测元素和内标元素响应值的比值线性关系良好(r≥0.9990);精密度、重复性、稳定性试验结果的RSD均小于4%(n=6);加样回收率为80.69%~99.85%,RSD为0.92%~4.03%(n=6)。20批样品中,主要含常量元素Ca,Na,Mg,K(>45 mg/kg),微量元素含量较多的为Fe,Zn,Al,Ba,B,Mo,重金属及有害元素Pb,As,Cd,Cu均未超标,Co和Hg元素均未检出。无机元素特征图谱整体相似,其中Ca,Zn,Fe,Cu,B 5种无机元素为不同批次连钱草的质量差异性成分。结论该方法操作简便、结果准确、重复性好,可用于连钱草药材中19种无机元素的含量测定及其质量评价。Objective To establish an inductively coupled plasma-mass spectrometry(ICP-MS)method for simultaneous determination of 19 inorganic elements[potassium(K),calcium(Ca),sodium(Na),magnesium(Mg),aluminum(Al),zinc(Zn),iron(Fe),manganese(Mn),selenium(Se),cadmium(Cd),lead(Pb),copper(Cu),boron(B),Cr(Cr),barium(Ba),mercury(Hg),molybdenum(Mo),cobalt(Co),and arsenic(As)]in Glechomae Herba,and to determine the chemical stoichiometry analysis method for the distribution characteristics of inorganic elements.Methods Microwave digestion was used for sample pre-treatment,the flow rate was set at 17 L/min for the plasma argon and 1.5 L/min for the carrier gas,the sampling depth was 11 mm,the temperature of the atomization chamber 3.0℃,the measurement mode was collision pool kinetic energy discrimination(KED)mode,the collision airflow was 6.5 mL/min,the injection flushing time was 45 s,and the peristaltic pump speed was 60 r/min.With scandium(45Sc),indium(115In),and bismuth(209Bi)as internal standards,the fingerprints of inorganic elements were established,and principal component analysis(PCA)and orthogonal partial least squares discriminant analysis(OPLS-DA)were used to evaluate its characteristic elements.Results The linear relationship between the response values of 19 inorganic elements within their respective mass concentration ranges and the measured elements/internal standard elements was good(r≥0.9990).The RSDs of precision,repeatability,and stability test results were all lower than 4%(n=6).The recovery rates of inorganic elements were in the range of 80.69%-99.85%,with RSDs of 0.92%-4.03%(n=6).Among the 20 batches of samples,the they mainly contained constant elements Ca,Na,Mg,K(>45 mg/kg),the elements with a high content of trace elements were Fe,Zn,Al,Ba,B,Mo,while the heavy metals and harmful elements Pb,As,Cd,Cu did not exceed the standard,and Co and Hg elements were not detected.The fingerprints of inorganic elements were generally similar,among which Ca,Zn,Fe,Cu,and B were the quality differential components of
关 键 词:连钱草 电感耦合等离子体质谱法 主成分分析 正交偏最小二乘法判别分析 无机元素 特征图谱
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