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藏药细果角茴香中16种微量元素含量测定与分析

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目的 为细果角茴香微量元素含量测定及规范种植提供参考。方法 采用电感耦合等离子体发射光谱(ICP-OES)法测定青海省不同产地27批样品中铝(Al)、钡(Ba)、钙(Ca)、钾(K)、镁(Mg)、锰(Mn)、钠(Na)、磷(P)、锶(Sr)、钛(Ti)、硼(B)、铁(Fe)、锂(Li)、钒(V)、锌(Zn)含量,等离子体射频发射功率为1。20 kW,等离子气流量为15L/min,雾化器流量为0。75 L/min,辅助气流量为1。5L/min,观察10 min,一次读数3 s,稳定15 s,等离子气、雾化气和辅助气均为高纯氩气,检测波长分别为396。2,455。4,317。9,766。5,279。6,257。6,589。6,213。6,407。8,336。1,249。8,238。2,670。8,292。4,213。9 nm。采用原子荧光光谱法测定硒(Se)含量,灯电流为 100 mA,屏蔽气流速为1 000mL/min,负高压为340 V,载气流速为500 mL/min,原子化器高度为8 mm,注入体积为2mL,载气、屏蔽气均为高纯氩气。采用主成分分析(PCA)和判别对应分析(DCA)各微量元素含量测定结果。结果 15种元素和Se质量浓度分别在0。02~10 μg/mL、0~40 μg/L范围内与峰面积线性关系良好(r>0。999 6);检测限分别为0。018~3。000 mg/L、0。002 mg/L;精密度、重复性试验结果的RSD均小于3。0%;平均加样回收率为94。01%~102。15%及91。44%,RSD均小于10%(n=6)。各批样品中16种元素的平均含量排序为 K>Ca>Mg>P>Na>Fe>Al>Sr>Zn>Mn>Ba>B>Ti>V>Li>Se。PCA 结果显示,Al、Fe、Li、Mn 是藏药细果角茴香的特征微量元素。DCA结果显示,Fe,Al,Ca,Ti,Mn,V,Ba含量与海拔呈正相关,与经纬度均呈负相关;K,Zn,Sr,Mg,Na、P含量反之;Se,Li,B含量与海拔、经纬度均无相关性。结论 建立的方法操作简便,结果稳定、可靠,可用于细果角茴香微量元素含量测定;青海省不同产地细果角茴香中各微量元素的含量差异较大,与产地海拔和经纬度有一定相关性。
Determination and Analysis of 16 Trace Elements in Tibetan Medicine Hypecoum Leptocarpum
Objective To provide a reference for the determination of trace element and standardized cultivation of Hypecoum leptocarpum.Methods The inductively coupled plasma-optical emission spectrometry(ICP-OES)method was used to determine the contents of aluminum(Al),barium(Ba),calcium(Ca),potassium(K),magnesium(Mg),manganese(Mn),sodium(Na),phosphorus(P),strontium(Sr),titanium(Ti),boron(B),iron(Fe),lithium(Li),vanadium(V)and zinc(Zn)in 27 batches of samples from different producing areas in Qinghai Province;the plasma radio frequency power was 1.20 kW,the plasma gas flow rate was 15 L/min,the atomizer flow rate was 0.75 L/min,the auxiliary air flow rate was 1.5 L/min,the observation time was 10 min,the single reading time was 3 s,the stabilization time was 15 s,the plasma gas,atomization gas and auxiliary gas were all high-purity argon,the detection wavelengths were 396.2,455.4,317.9,766.5,279.6,257.6,589.6,213.6,407.8,336.1,249.8,238.2,670.8,292.4,213.9 nm respectively.The atomic fluorescence spectrometry was used to determine the content of selenium(Se),the lamp current was 100 mA,the shielding gas flow rate was 1 000 mL/min,the negative high voltage was 340 V,the carrier gas flow rate was 500 mL/min,the atomizer height was 8 mm,the injection volume the 2 mL,the carrier gas and shielding gas were both high-purity argon.Principal component analysis(PCA)and discriminant correspondence analysis(DCA)were used to determine the content of various trace elements.Results The linear ranges of 15 elements and Se were 0.02-10 μg/mL and 0-40 μg/L respectively(r>0.999 6).The limits of detection(LOD)were in the range of 0.018 to 3.000 mg/L,0.002 mg/L respectively.The RSDs of precision and repeatability tests were both lower than 3.0%.The average recovery rates of 15 elements and Se were in the range of 94.01%to 102.15%,91.44%respectively,with the RSDs lower than 10%(n=6).The average content of 16 elements in each batch of samples was ranked as K>Ca>Mg>P>Na>Fe>Al>Sr>Zn>Mn>Ba>B>Ti>V>Li>Se.The PCA showed that Al,Fe,Li and Mn were the characteristic trace elements of Tibetan medicine Hypecoum leptocarpum.The DCA showed that Fe,Al,Ca,Ti,Mn,V,Ba contents were positively correlated with the altitude and negatively correlated with the longitude and latitude;while K,Zn,Sr,Mg,Na,P contents were the opposite;and Se,Li,B contents were not correlated with the altitude or longitude and latitude.Conclusion The established method is easy,stable and reliable,which can be used for the determination of trace element in Hypecoum leptocarpum.The content of various trace elements in Hypecoum leptocarpum from different producing areas in Qinghai Province varies greatly,and has a certain correlation with the altitude,longitude and latitude of the producing areas.

Hypecoum leptocarpumtrace elementcontent determinationaltitudelongitudelatitudeQinghai Province

吴雪花、金秉巾、丁玉、郑心悦、梁永欣、林鹏程、李生有

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青海省人民医院,青海西宁 810007

青海民族大学药学院·青海省青藏高原植物化学重点实验室·国家民委青藏高原藏药资源保护与开发利用重点实验室,青海西宁 810007

细果角茴香 微量元素 含量测定 海拔 经度 纬度 青海省

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(24)