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1.
建立了二维柱切换-超高效液相色谱法同时测定明目地黄丸中莫诺苷、马钱苷、芍药苷、丹皮酚含量的方法.一维色谱柱为Thermo Accucore XL C18(250mm×2.1 mm,4μm),二维色谱柱为DIONEX Acclaimphenyl-1(150mm ×4.6mm,3μm),一维分析流动相为乙腈-水,梯度洗脱,二维分析流动相为乙腈-水,等度洗脱,14.5 min进行阀切换;检测波长:0~14.5 min为240 nm,14.5~ 30 min为275 nm,流速:0.5 mL/min,柱温:30℃.30 min即可完成明目地黄丸中莫诺苷、马钱苷、芍药苷、丹皮酚的含量测定,并有效地将莫诺苷同分异构体分离.莫诺苷、马钱苷、芍药苷、丹皮酚的线性范围分别为7.6 ~ 377 mg/L,9.2~ 459 mg/L,8.4~419 mg,/L和8.2 ~ 409 mg/L,相关系数为0.9999,加样回收率为98.3%~ 100.2%.本方法快捷高效,可对控制明目地黄丸质量提供参考.  相似文献   

2.
橙汁类饮料中橙皮苷、柚皮苷含量的测定   总被引:1,自引:0,他引:1  
建立了反相高效液相色谱法测定橙汁中橙皮苷和柚皮苷的方法,并对不同厂家生产的橙汁饮料中橙皮苷和柚皮苷进行了比较.采用SHIMADZUVPODS(4.6 mm×150 nn,5μm)色谱柱;V(乙腈):V(磷酸水溶液)=22:78(pH 3.5)为流动相,流速为1.2 Ml/min;检测波长为283 nm.结果待测组分与其他组分分离度良好(>1.5),橙皮苷和柚皮苷线性范围分别为2.8~56.0 μg/mL和0.43~8.6μg/mL,橙皮苷和柚皮苷的平均回收率分别为99.9%,98.9%,RsD分别为1.9%,1.3%.  相似文献   

3.
建立了一种快速测定龙胆泻肝丸中栀子苷、龙胆苦苷和黄芩苷3种有效成分的超高效液相色谱方法。样品经50%甲醇提取,C18固相萃取(SPE)小柱净化后,采用Ultimate XB-C18色谱柱(4.6 mm×50 mm,1.8μm)进行分离,以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱。考察了不同规格色谱柱、流动相梯度比例、进样体积、柱温和流速对分离效果的影响,并对SPE柱流出液的平衡体积进一步考察,在最佳分析条件下进行液相色谱分析,该方法显示了良好的线性关系(r≥0.999 8),其定量下限(LOQ)为0.24~0.44 mg/L,加标回收率为95%~99%。该方法快速、准确,可满足实际检测需要。  相似文献   

4.
建立了微乳液相色谱(MELC)测定中药复方制剂清开灵注射液中黄芩苷含量的分析方法,并考察了微乳流动相的组成及pH值等影响因素.最佳条件为:采用Hypersil BDS C18 5 μm(4.6 mm×150 mm)色谱柱,柱温30 ℃,以3%十六烷基三甲基溴化铵-0.8%乙酸乙酯-7%乙腈-0.01 mol/L 四丁基溴化铵(磷酸调pH至3.0)为流动相,检测波长276 nm.对照品和样品均用70%甲醇处理.结果表明,黄芩苷的线性范围为25 ~100 mg/L,相关系数r=0.999 9.精密度实验和稳定性实验的RSD分别为1.0%(n=6)和0.50%(n=5),平均加标回收率和RSD值(n=6)分别为99%、1.9%.市售9批样品中黄芩苷的质量浓度为4.05 ~5.05 g/L,符合药典规定.  相似文献   

5.
HPLC测定河套大黄中的土大黄苷含量   总被引:3,自引:0,他引:3  
从河套大黄中分离纯化出活性成分土大黄苷,作为自制的标准品,利用KromasilTM C(18)(250 mm×4.6 mm I.d.,5μm)反相色谱柱,以V(甲醇):V(乙腈):V(水)=35:5:60为流动相,以320mm为检测波长,对河套大黄中土大黄苷进行测定.土大黄苷在0.427~4.190μg范围内与峰面积呈良好线性关系(r=0.9994),平均回收率为99.12%.该方法为河套大黄的质量控制奠定了基础.  相似文献   

6.
建立了高速逆流色谱分离制备防风中有效成分升麻素苷和5-O-甲基维斯阿米醇苷的方法.防风根的粉末经甲醇浸泡提取和减压蒸馏,得粗提浸膏.以V(乙酸乙酯):V(正丁醇):V(水)=2:7:9为溶剂,上相为固定相,下相为流动相,流速2.0 mL/min.从316 mg防风粗提物中一步分离得到13.9 mg升麻素苷和25 mg 5-O-甲基维斯阿米醇苷,纯度分别为98.1%和99 2%.采用ESI-MS, 1H NMR 和13C NMR对目标化合物的结构进行了鉴定.  相似文献   

7.
采用加压毛细管反相电色谱技术,建立了一种用于分离检测芎菊上清片中栀子苷和黄芩苷的高效简便新方法。色谱柱为EP-100-20/45-3 C18毛细管柱(总长度45 cm,有效长度20 cm,直径为100μm,ODS填料内径3μm),柱温为25℃,流动相采用20 mmol/L Na H2PO4-乙腈(71∶29),流动相的总流速为0.035m L/min,分离电压为+2.0 k V,检测波长为240 nm。经等度洗脱,栀子苷和黄芩苷可实现快速分离,峰面积的相对标准偏差(RSD)不大于2.8%,回收率为91.9%~101.2%,测得该芎菊上清片中栀子苷的含量为2.616 mg/g,黄芩苷的含量为11.220 mg/g。该方法的选择性好、柱效高、试剂用量少,用于芎菊上清片中黄芩苷和栀子苷的分离检测,结果满意。  相似文献   

8.
HPLC法同时测定红景天中红景天苷、酪醇和没食子酸   总被引:2,自引:0,他引:2  
用高效液相色谱法同时测定大花红景天中红景天苷、酪醇和没食子酸的含量.采用C18 (4.6 mm×200 mm,5 μm)色谱柱,V(甲醇)∶V(0.5%磷酸水溶液)=5∶95为流动相,流速1.0 mL/min,柱温40 ℃,在278 nm下进行检测.大花红景天中红景天苷、酪醇和没食子酸的平均含量分别为3.06%,0.78%和0.18%.平均回收率分别为99.90% (RSD=1.86%)、100.70% (RSD=0.74%)和99.10% (RSD=1.64%).该方法可用于测定红景天中红景天苷、酪醇和没食子酸的含量.  相似文献   

9.
提出了高效液相色谱-串联质谱法测定葛根中葛根素和大豆苷元的含量。样品经乙醇提取,所得提取液用乙醇定容至100mL后经Waters Xterra MS C18色谱柱(150mm×3.9mm,5μm)分离,用乙腈与50mmol.L-1甲酸溶液(40+60)的混合液洗脱,采用电喷雾正离子电离多反应监测模式。葛根素和大豆苷元的质量浓度分别在0.050~0.50mg.L-1和5.0~50mg.L-1之间与峰面积呈线性关系,检出限(3S/N)均为5μg.L-1。在0.1,1.0,10.0mg.L-1 3个浓度水平进行加标回收试验,葛根素和大豆苷元的回收率分别为96.6%和97.4%。  相似文献   

10.
毛细管电泳法检测甜菊糖条件的中心复合设计优化   总被引:1,自引:1,他引:0  
采用高效毛细管电泳分离并检测了甜菊叶中莱鲍迪苷A(RA)和斯替维苷(St)的含量.在单因素实验确定主要影响因素的基础上,用中心复合设计实验和响应面分析的方法对主要影响因素的取值进行了优化.优化后RA和St的分离度增大,迁移时间缩短,整体的分离检测效率得到了明显的提高.在含有23.7%(体积分数)乙腈和6.3%(体积分数)甲醇的52 mmol/L硼砂缓冲液(pH 10.10)中,RA和St在20 min内得到良好的分离.RA和St的质量浓度分别在0.10 ~5.0 g/L和0.30 ~5.0 g/L内与电泳峰高呈良好的线性关系,检出限分别为RA:0.01 g/L,St:0.02 g/L.该方法已成功地应用于实际样品的检测.  相似文献   

11.
多环芳二酐型聚酯亚胺膜的透气性能李悦生,丁孟贤,徐纪平(浙江大学高分子科学与工程研究所,杭州,310027)(中国科学院长春应用化学研究所)关键词聚醚酰亚胺,聚酯酰亚胺,膜,透气性通常的聚酰亚胺加工性能较差,在芳环二酐的苯环间引入醚键等柔性基团后,其...  相似文献   

12.
13.
A QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for the determination of benazolin-ethyl and quizalofop-p-ethyl in rape and soil by high-performance liquid chromatography-tandem mass spectrometry has been developed in this study. The residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil were determined with the developed method. The half-lives of benazolin-ethyl in rape straw and soil were 3.7–5.1 days and 14.3–26.3 days, respectively. The half-lives of quizalofop-p-ethyl in rape straw and soil were 5.0-6.1 days and 0.3–9.7 days, respectively. The residue of benazolin-ethyl and quizalofop-p-ethyl in rapeseed and soil were below the detection limit (i.e., 0.5?mg?kg?1, the maximum residue level of European Union for quizalofop-p-ethyl).  相似文献   

14.
微量元素与疾病诊断治疗的研究现状及展望   总被引:8,自引:0,他引:8  
对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述,包括:微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。  相似文献   

15.
Herein, we present the synthetic route and the photophysical, electrochemical as well as laser properties of novel red‐emitting boron‐dipyrromethenes (BODIPYs) bearing arylethyne moieties. Such functionality is added along the main axis of the chromophore leading to single‐ and double‐substituted derivatives. The relationship between the dye structure and the lasing properties is studied in detail with the help of the photophysical and electrochemical properties as well as quantum mechanical simulations. The asymmetric substitution of the parent dye induces inhomogeneities in the charge distribution, which leads to an overall loss of the fluorescence capacity, mainly in polar media. Such non‐radiative deactivation processes can be softened by decreasing the electron‐donor ability of the substituent or even avoided by symmetrical substitution. Thus, grafting of the arylethyne moieties at the longitudinal axis of the indacene core results in an effective strategy to develop red‐edge BODIPYs with highly efficient and photostable laser emission.  相似文献   

16.
In this work, ferrocene- and ferrocenium-containing salts were employed to modify montmorillonite. X-ray measurements show an increase in the interlayer spacing upon clay modification, which means that the larger and more organophilic cations were inserted into the gallery space of montmorillonite. Attempts to prepare nanocomposites of polystyrene and ethylene vinyl acetate copolymers lead to immiscible systems; the morphology of these systems was elucidated with TEM, XRD and cone calorimetry. The thermal stability of the composites is greater than that of the virgin polymer.  相似文献   

17.
The monomeric ν(N—H) vibrations of various trisubstituted ureas of the R2UPh type and -thioureas of the R2TUPh type have been studied. The trans—out isomerism in the former and the trans—out—cis isomerism in the latter are discussed from the point of view of steric effect. The monomeric ν(N—H) vibrations of RPhUPh and RPhTUPh are also examined. The single band appearing in the spectrum of both ureas is characteristic of the cis form; this suggests the existence of phenyl—phenyl interaction (the stacking interaction proposed by Galabov et al. [10]). Behavior of ν(N—H) vibrations at several concentrations is shown to be clearly different in the three forms (trans, out and cis). The presence of the cis form is confirmed by solvent effect experiments.  相似文献   

18.
朱劲波  马立群  梁飞  苗迎春  王立民 《应用化学》2015,32(11):1221-1230
Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB5型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。  相似文献   

19.
钒与糖代谢及糖尿病   总被引:1,自引:0,他引:1  
微量元素钒作为生物体内必需元素,经证实有很重要的生理学功能,与机体糖代谢有十分密切的关系,且能降低糖尿病动物模型的高血糖,极有可能被开发为治疗糖尿病的药物。  相似文献   

20.
Neutral nickel(II) and palladium(II) complexes bearing β-ketoiminato ligand have been synthesized. The two complexes have been investigated as catalyst for the polymerization. Using methylaluminoxane (MAO) as a cocatalyst, both complexes produce vinyl-addition polynorbornenes, but palladium(II) complex displays much higher activity up to 8.0 × 107 g/(molPd h). Furthermore, both Ni(II) and Pd(II)/MAO system can efficiently copolymerize norbornene and 5-norbornene-2-yl acetate (NB-OCOMe) in moderate yields and in relatively high molecular weights. The analyses of the product by FTIR, 1H NMR and 13C NMR spectra give the verification of vinyl addition copolymer. The copolymers show narrow molecular weight distribution and good solubility in common organic solvents.  相似文献   

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