ICP—AES法测定玫瑰花、金银花中多种微量元素

研究了用微波消解ICP—AES对玫瑰花、金银花中Cu、Zn、Fe、Mn、Na、Ca6种元素进行测定的方法,优化了ICP—AES的工作参数,考察了消解液的种类及用量对测定结果的影响,选择玫瑰花的消解液为V（HNO,）＋V（HClO4）：5＋3,金银花的消解液为V（HNO,）＋V（HClO4）=10＋3。结果表明,6种元素的检出限在0．005～0．021μg／mL之间,相对标准偏差（RSD）均小于8％,回收率为95．6％～103．9％,该法用于玫瑰花、金银花中元素的测定,结果令人满意。金银花、玫瑰花中含有丰富的微量元素,对人体健康十分有益。     

FAAS法测定三种中药材中的微量元素

采用V（浓硝酸）＋V（高氯酸）=4＋1混酸溶解消化样品。用火焰原子吸收光谱法（FAAS）测定了红芪、黄芪、板蓝根中K、ca、Na、Mg、Fe、Mn、Zn、Cu8种微量元素的含量。结果表明,红芪中钙的含量最高,铜的含量最低;黄芪和板蓝根中镁的含量最高,铜的含量最低。各元素回收率（n=7）在96．07％～101．26％之间,RSD值（n=7）在0．60％～2．99％之间。     

怀菊花中微量铁的测定

为探讨邻二氮菲分光光度法测定怀菊花中微量元素铁含量的可行性,怀菊花的药理功效、食用营养价值与微量元素含量可能存在的关系,根据铁离子与特定显色剂显色产生可见吸收,采用混合酸y（HNO3）：V（HClO4）=4＋1对怀菊花样品湿法消化处理,在pH2～9的溶液中试剂与铁生成稳定的橙色络合物,并用分光光度法测定了怀菊花中微量元素铁含量。结果表明,所选的怀菊花中铁含量303．9～337．9μg／g,加标回收率为90．2％～100．6％。分光光度法操作简便、干扰离子少,测量快速、结果准确度和灵敏度高,易推广和 普及使用。     

红薯中铜铁微量元素测定

目的：测定三个品种红薯（黄心红薯、白心红薯、紫红薯）中Cu、 Fe微量元素含量。方法采用V（硝酸）＋V（高氯酸）＝4＋1体系分解样品,火焰原子吸收光谱法（ FAAS）测定。结果黄心红薯、白心红薯、紫红薯中Cu、 Fe微量元素均含量丰富,其Cu含量由大到小次序为：紫红薯,黄心红薯,白心红薯, Fe含量的由大到小次序为：黄心红薯,白心红薯,紫红薯。回收率在99.00％～104.00％之间, RSD＜2.2％。结论测定结果可为进一步研究红署营养价值与微量元素的关系提供参考。     

火焰原子吸收法测定九管血不同部位的微量元素

为测定九管血的不同部位Fe、Cu、Mn、Zn的含量,样品用V（HNO3）＋V（HClO4）=4＋l进行消化处理,然后在实验选定的最佳工作条件下,用火焰原子吸收光谱法（FAAS）对九管血不同部位的Fe、Cu、Mn、Zn微量元素进行测定。结果表明,九管血根、茎、叶、籽中微量元素含量丰富,其中Fe含量最高,Cu含量最低,为九管血药效的进一步研究和资源综合开发利用提供一定的科学依据。     

补阴类中草药中四种微量元素的测定

为测定补阴类中药中Zn、Fe、Cu、Mn 4种微量元素的含量,采用V(HNO3)+V(HClO4)=4+1混合酸常压微沸条件下消解样品,运用火焰原子吸收光谱法测定了补阴类中草药女贞子、桑寄生、木蝴蝶中Zn、Fe、Cu、Mn 4种微量元素的含量。结果表明,3种中草药Fe含量最高,Zn、Mn次之,Cu含量最低。该法的加标回收率在95.2%～105.4%之间,RSD<2.000 0%,具有良好的准确度和精确度。结果为这类中药保健作用的进一步开发提供了参考。     

火焰原子吸收法测定中草药地胆草中微量元素的含量

目的运用火焰原子吸收光谱法测定中草药地胆草中的Fe、Zn、Mg、Ca、Cu5种微量元素的含量。方法用浓HNO3-HCIO4消解样品,采用标准曲线法测定其五种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素,Ca含量尤其丰富,高达12225μg／g。方法回收率在99．4％～104．0％之间,样品相对偏差小于5％。结论该法快速简便、重复性好、准确度好,适用于同类生物样品中微量元素的测定,结果令人满意。     

野生中草药木贼中微量元素的测定

目的测定中草药木贼中微量元素的含量。方法用湿法消化及于法灰化两种方法处理样品并进行了比较,用火焰原子吸收法测定了中草药木贼中7种微量元素的含量。结果测定结果湿法的RSD在0．5％～3．0％,干法的RSD在0．5％-7．5％之间。结论湿法处理金属离子损失小,测量精密度更好。木贼中微量元素的含量由高到低顺序为：Mg,Fe,Mn,Zn,Cu,Ph,Ni。     

容量法测定氧化钒中的各种价态钒

用NaOH溶液处理样品，分离V（V）然后以Fe(Ⅱ）滴定测定之。定量加入过量的V（V）到上述残渣中并用H2SO4溶解，用Fe(Ⅱ）滴定，计算出V（Ⅱ），V（Ⅲ）的含量。V（Ⅳ）的测定是通过从总钒量中扣除V（Ⅱ）、V（Ⅲ）、V（Ⅴ）的含量得到。V（Ⅱ）、V（Ⅲ）和V（Ⅴ）的回收率均大于96％，其8次测定结果的相对标准偏差分别为：9．8％、0．4％、1．2％；本法快速、简便，在实际应用中效果良好。     

火焰原子吸收法测定翼梗五味子中微量元素的含量

目的：运用火焰原子吸收光谱法测定中草药翼梗五味子藤中的 Fe、 Zn、 Mg、 Ca、 Cu 5种微量元素的含量。方法用浓 HNO3-HClO4消解样品,采用标准曲线法测定其5种金属元素含量。结果所测的样品中含有丰富的人体必需微量元素, Ca 含量尤其丰富,高达15827μg/g。方法回收率在99．7％～105．0％之间,样品相对偏差小于5％。结论该法快速简便、重复性好、准确度好,适用于同类生物样品中微量元素的测定,结果令人满意。     

五种中草药中七种元素含量测定研究

用火焰原子吸收法对五种中草药中K，Ca,Mg,Cu,Zn,Fe,Mn进行了测定，结果表明，这些元素与中药的药理作用有相关性。     

火焰原子吸收光谱法测定温里类中草药中痕量元素

应用火焰原子吸收光谱法测定了6种温里类中草药(即香附子、干姜、肉桂、细辛、高良姜及小茴香)中4种痕量元素铜、铁、锌及锰的含量。样品用硝酸-高氯酸(4+1)混合酸消解后加入过氧化氢,并蒸发至近干,残渣溶于硝酸(1+99)溶液中后用于火焰原子吸收光谱法分析,标准曲线分别用上述4种元素的标准溶液制作。按此方法分析了上述6种中草药中铜、铁、锌及锰4种痕量元素,并在此基础上用标准加入法作了回收试验,测得4种痕量元素的回收率在93.5%~109.0%之间。     

微波消解-高分辨连续光源原子吸收光谱法测定锁阳和韭菜籽中的重金属元素含量

利用微波消解-高分辨连续光源原子吸收光谱法测定锁阳、韭菜籽两种中药材中铜(Cu)、铅(Pb)、镉(Cd)、铬(Cr)、砷(As)和汞(Hg)的含量.采用微波消解进行样品前处理,火焰原子吸收法测定其中的Cu含量,石墨炉原子吸收法测定Pb、Cd和Cr含量,氢化物发生原子吸收法测定As、Hg含量.方法线性关系良好,相关系数R^2大于0.999,加标回收率为95.61%~100.1%,RSD为0.8%~3.3%,测得锁阳和韭菜籽中Cu、Pb、Cd、Cr、As和Hg的含量值均低于《药用植物及制剂进口绿色行业标准》和食品安全国家标准《食品中污染物限量》(GB2762-2012)中规定的限量指标.方法分析速率快、干扰少、精密度高,适用于中药材中重金属含量的测定.     

Quality assessment of crude and processed ginger by high‐performance liquid chromatography with diode array detection and mass spectrometry combined with chemometrics

A sensitive, simple, and validated high‐performance liquid chromatography with diode array detection and mass spectrometry detection method was developed for three ginger‐based traditional Chinese herbal drugs, Zingiberis Rhizoma, Zingiberis Rhizome Preparatum, and Zingiberis Rhizome Carbonisata. Chemometrics methods, such as principal component analysis, hierarchical cluster analysis, and analysis of variance, were also employed in the data analysis. The results clearly revealed significant differences among Zingiberis Rhizoma, Zingiberis Rhizome Preparatum, and Zingiberis Rhizome Carbonisata, indicating variations in their chemical compositions during the processing, which may elucidate the relationship of the thermal treatment with the change of the constituents and interpret their different clinical uses. Furthermore, the sample consistency of Zingiberis Rhizoma, Zingiberis Rhizome Preparatum, and Zingiberis Rhizome Carbonisata can also be visualized by high‐performance liquid chromatography with diode array detection and mass spectrometry analysis followed by principal component analysis/hierarchical cluster analysis. The comprehensive strategy of liquid chromatography with mass spectrometry analysis coupled with chemometrics should be useful in quality assurance for ginger‐based herbal drugs and other herbal medicines.     

Establishment of a search library about benzylisoquinoline alkaloids based on selective separation on the binaphthyl column and standard analysis on C18 column

A search library about benzylisoquinoline alkaloids was established based on preparation of alkaloid fractions from Rhizoma coptidis, Cortex phellodendri, and Rhizoma corydalis. In this work, two alkaloid fractions from each herbal medicine were first prepared based on selective separation on the “click” binaphthyl column. And then these alkaloid fractions were analyzed on C18 column by liquid chromatography coupled with tandem mass spectrometry. Many structure‐related compounds were included in these alkaloids fractions, which led to easy separation and good MS response in further work. Therefore, a search library of 52 benzylisoquinoline alkaloids was established, which included eight aporphine, 19 tetrahydroprotoberberine, two protopine, two benzyltetrahydroisoquinoline, and 21 protoberberine alkaloids. The information of the search library contained compound names, structures, retention times, accurate masses, fragmentation pathways of benzylisoquionline alkaloids, and their sources from three herbal medicines. Using such a library, the alkaloids, especially those trace and unknown components in some herbal medicine could be accurately and quickly identified. In addition, the distribution of benzylisoquinoline alkaloids in the herbal medicines could be also summarized by searching the source samples in the library.     

“浙八味”药材中重金属铅、镉、铜含量分析

为对"浙八味"药材质量控制和安全用药提供可靠的依据,采用灰化法处理样品,火焰原子吸收分光光度法测定了其铅、镉、铜含量。结果表明,8种药材中的铅含量为0.828 1~1.747 3 mg.kg-1,镉含量为0.116 9~0.295 0mg.kg-1,铜含量为2.519 5~8.286 4 mg.kg-1。8种药材均检出一定量的有害重金属,但含量较低,未超出国家限量标准,符合《药用植物及制剂进出口绿色行业标准》的有关规定。     

微波辅助提取-气相色谱法同时测定中草药中有机磷和氨基甲酸酯农药残留

建立了中草药中有机磷和氨基甲酸酯类农药同时检测的气相色谱分析新方法.中药材试样依据正交实验的优化条件,用正己烷-丙酮(1∶4,V∶V)混合提取剂进行微波辅助提取,经弗罗里硅土和中性氧化铝混合层析柱净化后,采用HP-5毛细管柱分离,氮磷检测器同时检测中草药中15种有机磷和6种氨基甲酸酯类农药残留量.21种农药在0.01～1.0 mg/L的浓度范围内线性良好,线性相关系数为0.9950～1.000,检出限为0.002～0.01 mg/L.在0.05、0.2、0.5 mg/kg三个添加水平的平均回收率分别为75.11%～128.57%、75.85%～120.71%和76.43%～117.25%,相对标准偏差分别为 3.10%～10.58%、5.27%～9.94%和4.03%～9.03%.方法用于中草药中有机磷和氨基甲酸酯类农药残留的同时检测,结果良好.     

Elemental composition of herbal medicines sold over-the-counter in São Paulo city,Brazil

In Brazil, the use of herbal medicines is very popular due to its immense flora, cultural aspects and to the popular belief that herbs, which are of natural origin, are safe and without undesirable side effects. Aside from that public interest in natural therapies, the use of herbal medicines has increased expressively due to the high cost of synthetic medicines. In this study, elemental compositions of herbal medicines from the species Ginseng, Ginkgo biloba, Centella asiatica, Mulberry and Aloe vera supplied by different suppliers were evaluated by neutron activation analysis. The concentrations of As, Ba, Br, Ca, Cl, Co, Cr, Cs, Fe, Hf, K, Mg, Mn, Na, Rb, Sb, Sc, Th, Zn and some lanthanides were determined in these samples. Comparisons made between the results indicated differences in their elemental contents depending on the plant species, origins of the samples and the age of the leaves. The results also showed that the herbal medicines contain elements such as Ca, Co, K, Fe, Mg and Zn known as essential to humans and for treatment and prevention of diseases. Toxic elements such as Hg, Cd and Cu were not detected. Elements As and Sb were detected in some samples but at very low concentrations at the μg kg⁻¹ levels. Herbal medicine results were also compared to literature values. Biological certified reference material was analyzed for quality control of the analytical results.     

五种中药中微量元素及重金属元素的含量分析

用微波消解-原子吸收分光光度法对巴戟天、大黄、陈皮、板蓝根、茯苓等5种中药材中的7种金属微量元素进行了含量分析。结果表明,该法的线性良好,重现性在3.3%~11%之间,精密度在2.6%以内,回收率满足定量分析要求;5种药材中铅均未超标,茯苓中镉超出国家标准;5种药材里的铜含量均有超标,其中,巴戟天超标最严重;铁在5种药材中的含量最高,其中以巴戟天含量最为丰富,达到了746.750 mg/kg,其次是锌和锰,铬的含量最少。结论:对5种药材中铜均出现超标,虽然在边缘位置,但应该予以重视;巴戟天中丰富的铁元素,可能在防止癌变发生和发展中起到一定功效。