高效液相色谱化学发光抑制检测法测定烟草中的绿原酸和芸香苷

1 引言绿原酸和芸香苷是烟草中含量最多、最重要的多酚类化合物,发展绿原酸和芸香苷的高灵敏度和高选择性的分析方法对于烟叶质量的控制、植物生理的研究具有重要意义.基于绿原酸、芸香苷对鲁米诺化学发光的抑制作用,首次建立了绿原酸、芸香酸的高效液相色谱化学发光抑制检测法.该法灵敏度高、选择性好,用于烟草样品中绿原酸与芸香苷的测定,结果令人满意.     

毛细管电泳法测定复方鱼腥草片中的绿原酸和槲皮素

建立了毛细管电泳法分析复方鱼腥草片中绿原酸和槲皮素的方法,通过研究缓冲溶液酸度和浓度、工作电压和进样时间的影响优化了分析条件。在优化的条件下,15min内实现了两种分析物质的良好分离。绿原酸和槲皮素峰高和质量浓度分别在0．05～0．80g／L和0．05～1．00g／L范围内成良好线性。基于迁移时间和峰高的重复性(RSD)分别为：绿原酸,1．91％和4．32％;槲皮素,2．30％和3．18％。绿原酸和槲皮素的检出限(S／N=3)分别为0．014g／L和0．015g／L。通过分析实际样品并做加样回收实验进一步验证了该方法的可行性。     

HPLC柱切换技术用于同时分析鱼腥草中3种黄酮类成分

利用柱切换技术解决了鱼腥草中难分离组分的分离和低含量组分的定量问题。以Synergi Fusion-RP柱(250 mm×4.6 mm i.d.,4μm)作为预柱,甲醇-0.05%磷酸溶液作流动相,以Acclaim120 C18柱(250mm×4.6 mm i.d.,5μm)作为分析柱,乙腈-0.05%磷酸溶液作流动相,对鱼腥草中的3种黄酮类成分进行分析。该方法在10.0～1 000.0 mg.L-1范围内线性关系良好,相关系数(r)不低于0.998,回收率为95%～99%,RSD值均小于3%。该方法操作简便、快速,可作为分析鱼腥草中黄酮类组分的有效手段。     

HPLC法同时测定24种花中的5种活性成分含量

建立了高效液相色谱法(HPLC)同时测定24种花中绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素含量的方法。采用C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.2%冰乙酸溶液梯度洗脱,检测波长350 nm,柱温35℃,流速0.8 mL/min。绿原酸、金丝桃苷、槲皮素、木犀草素和异鼠李素分别在0.0208~104.00μg/mL(r=0.99993),0.017~85.00μg/mL(r=0.99998),0.0172~86.00μg/mL(r=0.99997),0.0304~152.00μg/mL(r=0.99997),0.0168~84.00μg/mL(r=0.99986)范围内与峰面积呈良好的线性关系,平均加标回收率(n=9)92.26%~99.09%,仪器精密度(n=6)RSD均小于3.1%,方法重复性(n=6)的RSD均小于3.6%。方法可同时测定这24种花中绿原酸和黄酮类物质的含量,可作为花中活性成分定量分析的方法。     

高效液相色谱法同时测定鱼腥草芩蓝合剂中7种成分

建立同时测定鱼腥草芩蓝合剂中绿原酸、连翘酯苷A、黄芩苷、槲皮苷、汉黄芩苷、槲皮素和汉黄芩素含量的高效液相色谱法.选择Symmetry Shield RP18色谱柱(4.6 mm×250 mm,5μm),以乙腈–0.1％磷酸溶液为流动相,梯度洗脱,检测波长为210 nm,柱温为30℃,进样体积为5μL.绿原酸、连翘酯苷A...     

无花果叶中有效成分鉴别及含量测定

近年来,无花果叶片中所含成分分析主要集中在同类型物质或整类物质,而对多种类型单一有效物质的定性定量研究较少。 本文采用溶剂浸提-超声波辅助法对无花果叶片中的有效成分进行了提取,利用气相色谱-质谱和超高效液相色谱-离子阱质谱对有效成分进行了鉴定。 结果表明,无花果叶中主要成分为绿原酸、芦丁、补骨脂素和佛手苷内酯。 采用单因素实验法,确定了4种成分的最佳提取工艺。 利用高效液相色谱建立了绿原酸、芦丁、补骨脂素和佛手苷内酯的定量分析方法。 绿原酸在1.84~9.2 μg范围内有良好的线性关系(R²=0.9991),回收率为95.2%;芦丁在3.4~17 μg范围内有良好的线性关系(R²=0.9981),回收率为96.8%;佛手内脂在4~20 μg范围内有良好的线性关系(R²=0.9998),回收率为89.5%;补骨脂素在4~20 μg范围内有良好的线性关系(R²=0.9963),回收率为87.1%。     

高效液相色谱法测定动物组织中鱼腥草素同系物含量

以氢氧化钠水解合成鱼腥草素类药物,然后用乙醚提取,除去乙醚后,用HPLC法测定大鼠血样和组织样品中药物的含量。结果表明:碱水解后合成鱼腥草素,形成共轭双键的烯醇式烷酰乙醛,紫外吸收显著增强,HPLC图谱测定物峰分离良好。血液加样标准曲线回归线性良好,r=0.999以上,线性范围为0.1-100mg/L,标准加入回收率为97.3%。利用该方法分析合成鱼腥草素类药物在动物血液、脑、肝、心脏、肾脏和肌肉等组织中的残留完全可行。     

高效液相色谱（HPLC）测定芦丁纯度和含量

研究了一种用于芦丁含量测定与纯度检验的高效液相色谱法（ＨＰＬＣ），该法具有较高精度和良好专属性，适于例行分析，分离在Ｃ８柱上进行，流动相为ＴＨＦ（四氢呋喃）－磷酸缓冲液，检测波长为２８０ｎｍ，检测限为０．５μｇ／ｍＬ，可检出０．０５％的杂质用于某些实际样品分析，结果良好。     

鱼腥草中钛含量分析方法研究

The research of the effects of surfactants on coloring reaction between titanium and phenyl fluorone was developed.A survey of coexisting elements in the houttuynia cordata thunb was carried out by X-ray fluorescence spectrometry,and a series of interference tests and analyses were performed.The interference can be eliminated by processing through high temperature cineration and adding ascorbic acid.A new method of determination of titanium in houttuynia cordata thunb was established by phenyl fluorone spectrophotometry in the presence of Emulsifier OP.The results showed that Beer's law is obeyed within the range of 0～0.32 μg·mL-1 for titanium.The relative standard deviation(RSD) was 1.9%～2.0%,and the recovery was 96.8%～100.6%.The method was applied for determination of titanium in houttuynia cordata thunb with satisfactory results.     

HPLC测定复方双花口服液中绿原酸和连翘苷的含量

复方双花口服液由金银花、连翘、板蓝根等用科学方法提取有效成分精制而成 ,主治各类因金黄色葡萄球菌所致感染性疾患。绿原酸和连翘苷是该制剂中主要有效成分。我们采用十八烷基硅烷键合硅胶色谱柱 ,对该口服液中绿原酸和连翘苷含量进行同时测定 ,结果准确 ,重现性好 ,可用于复方双花口服液的质量控制     

Simultaneous determination of eight active components in Houttuynia cordata injection and its quality control in productive process

A simple, reliable and effective gas chromatography coupled with flame ionization detection method was developed for the simultaneous determination of eight components (α‐pinene, β‐pinene, myrcene, limonene, terpinen‐4‐ol, α‐terpineol, bornyl acetate and methyl‐n‐nonylketone) in Chinese medicine Houttuynia cordata and its injection. The chromatographic separation of all eight components, including undecylene as internal standard was performed on a DB‐1 column (30 m×0.25 mm, 0.25 μm). Excellent linear behaviors including herb and injection over the investigated concentration ranges were observed with the values of r² higher than 0.9990 for all analytes. Satisfactory intra‐day and inter‐day precisions were achieved with RSD less than 2% and the average recoveries for all analytes at three different concentrations obtained were in the range of 93.4–104.4%, with RSD ranging from 1.3 to 4.1%. The proposed method was successfully applied in the simultaneous determination of these active components in H. cordata and H. cordata injection (HCI), including the intermediate product of HCI in productive process, from different pharmaceutical factories and different production batches, indicating that the method in this paper was particularly suitable for the routine analysis of HCI and its quality control in productive process.     

高效液相色谱法同时测定厚朴温中胶囊中的7种有效成分

建立了同时测定厚朴温中胶囊中山姜素、甘草酸、和厚朴酚、小豆蔻明、木香烃内酯、去氢木香内酯及厚朴酚含量的反相高效液相色谱法。固定相为Scienhome C18柱(250 mm×4.6 mm,5 μm),流动相为甲醇-乙腈-0.06%磷酸溶液(体积比为38∶27∶35),流速为1.0 mL/min,柱温为30 ℃,检测波长为235 nm。在上述条件下,山姜素、甘草酸、和厚朴酚、小豆蔻明、木香烃内酯、去氢木香内酯及厚朴酚的质量浓度分别在0.885～17.7,107～2140,8.85～17.7,1.035～20.7,4.85～97,5.9～118和17.5～350 mg/L时与色谱峰面积之间的线性关系良好;回收率分别为96.9%～101.1%,96.0%～100.5%,100.3%～100.8%,97.7%～101.4%,100.4%～102.3%,96.0%～102.3%和96.2%～100.6%。该方法简便、快速、准确,可用于厚朴温中胶囊的质量控制。     

水蒸汽蒸馏条件下鱼腥草中癸酰乙醛的高效提取及质谱定性

根据质谱学规律,剖析了在电子轰击下中药材鱼腥草中最关键的抗菌成分鱼腥草素(癸酰乙醛)的离子形成机理:癸酰乙醛的分子中存在两个-C=O,处于端位上的-C=O活性远大于-CH3,易失去H2O(M+-18)、CO(M+-28)等基团,产生较强的m/z180、170等离子碎片,此外,还易失去H2O+H2O(M+-36)、H2O+CO(M+-46)、CO+CO(M+-56)等基团,产生m/z162、152、142等离子碎片,这同实验中得到的癸酰乙醛质谱图完全吻合,纠正了文献中对癸酰乙醛的错误定性。在此基础上采用常规、Ar气保护和减压三种水蒸汽蒸馏方式提取鱼腥草挥发油,发现在惰性气氛或较低温度下有利于癸酰乙醛的提取,与常规水蒸汽蒸馏条件相比,Ar气保护下癸酰乙醛的含量从0.03%提高至0.53%,而减压条件下癸酰乙醛的溶出效率进一步提高至3.37%。研究表明常规水蒸汽蒸馏条件下癸酰乙醛易氧化分解是得到较少癸酰乙醛的根本原因。     

高效液相色谱-蒸发光散射检测法同时测定四君子丸中的5种有效成分

建立了同时测定四君子丸中党参炔苷、茯苓酸、甘草酸、苍术内酯III和白术内酯I含量的高效液相色谱法。色谱条件为: HIQ SIL C18 V色谱柱(250 mm×4.6 mm, 5 μm),以0.5%冰乙酸-甲醇体系为流动相进行梯度洗脱,流速为1.0 mL/min,采用蒸发光散射检测器检测,进样量为10 μL,柱温为25 ℃,漂移管温度为55 ℃,喷雾器加热级别为60%,载气为氮气,压力0.2 MPa。在上述条件下,党参炔苷、茯苓酸、甘草酸、苍术内酯III和白术内酯I的质量浓度分别在0.076～1.21, 0.048～0.76, 0.153～2.45, 0.045～0.72和0.098～1.56 g/L时,质量浓度的对数值与色谱峰面积的对数值之间的线性关系良好;平均回收率在97.13%～100.25%之间,相对标准偏差在1.23%～2.44%之间。该方法简便、快速、准确,可用于四君子丸的质量控制。     

鱼腥草中黄酮类成分的高效液相色谱指纹图谱分析

采用均匀实验设计和信息理论评价方法,建立了鱼腥草中黄酮类成分的高效液相色谱(HPLC)指纹图谱的分析方法。采用建立的方法和本研究室提出的指纹图谱评价软件,对同样种植条件下10个批次的鱼腥草指纹图谱进行了相似性评价,相似度均大于0.90;同时测定了芦丁、槲皮甙和槲皮素3个成分在10批鱼腥草药材中的含量分别为0.25%～0.34%、0.27%～0.37%、0.012%～0.016%。另外对不同采收季节和不同部位的鱼腥草药材中的黄酮类成分进行了指纹图谱的测定、主成分分析以及成分含量测定,结果表明,不同季节、不同部位的鱼腥草中黄酮类化合物的指纹图谱及成分含量存在较大的差异,且药用部位的差异大于采收季节的差异。该方法为规范鱼腥草中黄酮类成分在制药和用药的实际应用提供了一些可靠的基础信息。     

Simultaneous determination of three components by X-ray spectrometry after neutron activation

A method is described for the simultaneous determination of cadmium, antimony and praseodymium by 14-MeV neutron activation analysis based on characteristic X-ray spectrometry. The results of analysis show a relative error not higher than ±5%, when diluted with H₃BO₃ /90%/ and utilizing the internal standard method to minimize the interelement effects.     

Establishment of GC-MS fingerprint of fresh Houttuynia cordata

Fresh Houttuynia cordata THUNB. is a Chinese materia medica generally used in Chinese medicine therapy. It possesses the actions of clearing heat, eliminating toxins, reducing swelling, discharging pus and relieving stagnation. However, dry H. cordata has traditionally been used in clinical application instead of the fresh counterpart. In this paper, the chemical profiles of H. cordata were established using fingerprinting techniques. A modified GC-MS method was developed in the comparison of fingerprints among fresh and dry herbs of H. cordata. It was shown that the varieties, as well as relative levels of chemical components, in the fresh herb were more abundant than in the dry counterpart. Fingerprinting profiles were found to be consistent for fresh herbs acquired from various production areas, but the relative abundance of peaks were varied. Besides, the chemical components among different medicinal portions of fresh herbs were found to be inconsistent. The developed fingerprint can be successfully applied to distinguish between fresh and dry herbs, as well as determining differentiation among different medicinal portions.     

Establishment of HPLC-DAD-MS fingerprint of fresh Houttuynia cordata

A HPLC-DAD-MS fingerprint method of fresh Houttuynia cordata THUNB. was developed basing on the consistent chromatographic features among 11 batches of authentic samples. Major chemical components including phenolic compounds, flavones and alkaloids were simultaneously analyzed. Eleven common peaks in the fingerprint were chosen and identified by comparing their UV and ESI-MS data with the authentic compounds. The unique properties of this HPLC-DAD-MS fingerprint were successfully applied to analyze and differentiate samples from different geographical origins, processing methods and various medicinal parts of H. cordata. The results showed that these variations will give rise to differences in identities and/or abundance of chemical compounds, indicating that a comprehensive quality evaluation of those major ingredients in H. cordata is critical to assess and represent its overall quality.     

高效液相色谱-质谱法同时测定清热解毒口服液中的5种有效成分

建立了同时测定清热解毒口服液中的绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红5种有效成分的高效液相色谱-电喷雾电离质谱（HPLC-ESI/MS）分析方法。采用Zorbax SB C18色谱柱,以含0.2%甲酸的0.4 mmol/L醋酸钠(A相)、乙腈(B相)为流动相进行梯度洗脱,在ESI正离子模式下,采用选择离子监测方法进行测定,用峰面积进行定量。结果表明,绿原酸、栀子苷、黄芩苷、连翘苷和靛玉红的线性范围分别为0.050～50 mg/L,0.020～20 mg/L,0.005～30 mg/L,0.010～15 mg/L和0.010～10 mg/L;检出限分别为0.010,0.005,0.001,0.002和0.003 mg/L。5种成分的加样回收率为97.0%～101.7%,相对标准偏差小于2.2%。该法快捷、准确、重复性好,可用于清热解毒口服液中的5种有效成分含量的同时测定。