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HPLC测定秦艽中的生物碱和龙胆苦苷 总被引:4,自引:0,他引:4
目的建立同时测定秦艽中秦艽甲素、秦艽丙素和龙胆苦苷含量的方法。方法采用HPLC法。结果秦艽甲素在3.28~16.92μg内线性关系良好(R2=0.9991),平均加样回收率为94.42%,RSD=2.04%;秦艽丙素在0.05~4.87μg内线性关系良好(R2=0.9994),平均加样回收率为95.87%,RSD=1.66%;龙胆苦苷在79~390μg内线性关系良好(R2=0.9994),平均加样回收率为92.86%,RSD=2.19%。结论该法简便、准确、重复性好,为秦艽药材的评价提供了含量测定方法。 相似文献
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摘 要 目的:建立一测多评(QAMS)法测定六味五灵片中连翘苷、五味子醇甲、五味子酯甲、五味子甲素、五味子乙素和五味子丙素等6种有效成分的含量,验证该方法在制剂中应用的准确性和可行性。方法: 采用HPCL法,在230nm检测波长下建立五味子甲素与五味子乙素、五味子丙素、五味子酯甲、五味子醇甲和连翘苷的相对校正因子(f),计算六味五灵片中各成分的含量,实现一测多评。同时采用外标法测定,并计算QAMS法含量计算结果(Wf)和外标法含量测定结果(Ws)的相对误差,验证一测多评法的准确性,并对其重现性进行考察。结果: 建立用于测定六味五灵片中6种成分含量的QAMS法,并对10批制剂中六味五灵片的指标成分进行测定,其计算值与测定值的差异较小(RSD<5%)。结论:QAMS法用于测六味五灵片6种有效成分的含量,方法简单、有效、结果准确。QAMS法测六味五灵片的质量评价模式得到了验证,可用于六味五灵片的质量控制,并为后续的一测多评的研究提供参考价值。 相似文献
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摘 要 目的:建立雷公藤口服液中雷公藤甲素、总二萜内酯以及总生物碱的含量测定方法,为质量控制提供依据。 方法: 采用高效液相色谱(HPLC)法,Eclipse XDB C18色谱柱(150 mm×4.6 mm,5 μm),以乙腈 水为流动相进行梯度洗脱,流速1.0 ml·min-1,柱温40℃,检测波长218 nm,测定雷公藤口服液中雷公藤甲素的含量。采用紫外可见分光光度法,分别以雷公藤甲素、雷公藤次碱为对照,测定雷公藤总二萜内酯、总生物碱的含量。结果: 雷公藤甲素、总二萜内酯(以雷公藤甲素计)和总生物碱(以雷公藤次碱计)的线性关系良好(r≥0.999 8),平均加样回收率分别为91.96%、90.73%、99.18%,RSD均小于3%。结论:本研究所建立的方法稳定可靠,重复性良好,可用于雷公藤口服液的质量控制。 相似文献
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摘 要 目的:建立HPLC梯度法同时测定复方三七维康胶囊中三七皂苷R1、人参皂苷Rb1、Rg13种皂苷的含量。方法: 色谱柱:大连Spherisorb C18分析柱(200 mm×4.6 mm,5 μm);流动相:乙腈-水,梯度洗脱;流速:1.0 ml·min-1;检测波长 203 nm。结果:三七皂苷R1、人参皂苷Rg1和Rb1分别在1.06~18.55 μg(r=0.997 3)、2.02~35.35 μg(r=0.998 2)和2.02~35.35 μg(r=0.998 2)之间线性关系良好。平均回收率三七皂苷R1为100.8%(RSD=1.53%,n=5),人参皂苷 Rg1为98.9%(RSD=1.87%,n=5),人参皂苷Rb1为99.7%(RSD=1.90%,n=5)。结论:HPLC梯度洗脱法能够将多种皂苷很好地分离检测,该方法准确可靠,重复性好,可用于控制其质量。 相似文献
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目的 建立HPLC测定鱼腥草芩蓝合剂中绿原酸、黄芩苷和黄芩素的含量。方法 采用Kromasil-100 C18色谱柱(4.6?mm×250 mm,5 μm),流动相为甲醇-0.2%磷酸梯度洗脱,流速为1.0 mL·min-1,检测波长为322 nm,柱温为35 ℃。结果 绿原酸、黄芩苷和黄芩素线性范围分别为0.022 4~1.12 μg(R2=0.999 7),0.045 8~2.29 μg(R2=0.999 5)和0.031 8~ 1.59?μg(R2=0.999 9);3种成分的平均回收率分别为99.45%(RSD=1.4%),99.37%(RSD=2.0%)和97.90%(RSD=1.7%)。结论 本方法快速简便,精密度高,稳定性和重复性好,可用于鱼腥草芩蓝合剂中绿原酸、黄芩苷和黄芩素3种成分的定量分析和药品质量控制。 相似文献
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双波长薄层扫描法测定湖北贝母中湖贝甲素的含量 总被引:2,自引:0,他引:2
湖北贝母为百合科植物Fritillaria hupehensis Hsiao et K.C.Hsia的干燥鳞茎,拟收载于《中国药典》2000年版,为了控制药材质量,本文采用双波长薄层扫描法测定了湖北贝母中湖贝甲素(Hupehenine)的含量,用冷浸法提取,以苯-乙醚-醋酸乙酯-二乙胺(3:3:4:1)为展开剂,喷以稀碘化铋钾试液,双波长反射法锯齿扫描,λ_S=500nm,λ_R=600nm,回收率为101.4%,RSD=4.4%,经测定9批样品,含量为0.028%~0.187%,表明不同产地样品含量差异较大,建议暂订湖北贝母中湖贝甲素含量应不低于0.03%。 相似文献
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葛根中异黄酮含量的薄层光密度法测定 总被引:16,自引:0,他引:16
本文报道了葛根中异黄酮成分含量的薄层光密度测定法。用甲苯—甲醇—10%甲酸(7:3:0.02)和乙酸乙酯—甲醇—50%甲酸(8:2:0.2)为展开剂,在硅胶G薄层上分离了大豆甙元、大豆甙、葛根素和大豆甙元-4′,7-二葡萄糖甙,并用CS-910双波长薄层扫描仪进行了定量测定。变异系数为1.5~1.6%,采用本法测定了生药和片剂样品的含量。 相似文献
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秦皮中香豆素成分的薄层分离和光密度法测定 总被引:3,自引:0,他引:3
秦皮的乙醇提取液在硅胶G薄板上,用氯仿—甲醇—水(30:10:3)的下层25ml加甲酸0.5ml为展开剂,成功地分离了七叶亭、七叶灵、梣皮亭、梣皮甙和宿柱白蜡甙五种香豆素甙和甙元。用岛津CS-910型双波长薄层扫描仪测定其含量。对定量前薄板上分开的组分的定性进行了探讨。测定方法快速、灵敏、稳定、简便,为评价秦皮质量提供了有效的定量方法。 相似文献
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薄层荧光扫描法测定小叶买麻藤等植物中类化合物含量 总被引:4,自引:0,他引:4
目的 建立小叶买麻藤中6种类化合物的含量测定方法。方法 在高效硅胶薄层板上,买麻藤丙素、ε-viniferin、白藜芦醇、异丹叶大黄素、银松素以甲苯-冰醋酸-甲醇(3∶1∶0.2)为展开剂,进行二次展开;异丹叶大黄素-3-O-β-D-吡喃葡糖苷以甲苯-乙酸乙酯-冰醋酸-甲醇(1∶2∶0.5∶0.2)为展开剂,一次展开,展开后用液体石蜡-正己烷(1∶1)浸板,荧光扫描法测定。结果 6种化合物的线性关系良好,相关系数在0.9914~0.9999,回收率为94.4%~104.8%,RSD在2.3%~5.1%之间。用此法测定了小叶买麻藤等12种药用植物中此类化合物的含量和分布。结论 为研究和开发含类化合物的药用资源提供了简便、灵敏、准确的含量测定方法。 相似文献
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本文研究了影响麦角新碱、麦角胺和麦角毒碱的氧化铝薄层层离的各种因素.实验结果表明,酸性、中性和弱碱性氧化铝均能使三种麦角生物碱分离.氧化铝细度以小于200号筛的层离效果最好,莹光点圆而集中.苯-无水乙醇(10:0.5)是较为理想的推进剂,不仅分离效果好,而且其组成简单,容易处理和回收.层离板的斜度对层离效果影响不大,但以8—16°角较合适.层离槽放入溶剂后,必须先密闭放置10分钟,才能进行层离,否则容易产生边缘效应.根据以上研究桔果,制订了鉴定麦角中三种主要生物碱的方法. 相似文献
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Ergot sclerotia effect cereal crops intended for consumption. Ergot alkaloids within ergot sclerotia are assessed to ensure contamination is below safety standards established for human and animal health. Ergot alkaloids exist in two configurations, the R and S-epimers. It is important to quantify both configurations. The objective of this study was to validate a new ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method for quantification of six R and six S-epimers of ergot alkaloids in hard red spring wheat utilizing deuterated lysergic acid diethylamide (LSD-D3) as an internal standard. Validation parameters such as linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effects, recovery and precision were investigated. For the 12 epimers analyzed, low LOD and LOQ values were observed, allowing for the sensitive detection of ergot epimers. Matrix effects ranged between 101–113% in a representative wheat matrix. Recovery was 68.3–119.1% with an inter-day precision of <24% relative standard deviation (RSD). The validation parameters conform with previous studies and exhibit differences between the R and S-epimers which has been rarely documented. This new sensitive method allows for the use of a new internal standard and can be incorporated and applied to research or diagnostic laboratories. 相似文献
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Ruin Moaddel Galia Abdrakhmanova Joanna Kozak Krzysztof Jozwiak Lawrence Toll Lucita Jimenez Avraham Rosenberg Thao Tran Yingxian Xiao Carlos A. Zarate Irving W. Wainer 《European journal of pharmacology》2013,698(1-3):228-234
The effect of the (R,S)-ketamine metabolites (R,S)-norketamine, (R,S)-dehydronorketamine, (2S,6S)-hydroxynorketamine and (2R,6R)-hydroxynorketamine on the activity of α7 and α3β4 neuronal nicotinic acetylcholine receptors was investigated using patch-clamp techniques. The data indicated that (R,S)-dehydronorketamine inhibited acetylcholine-evoked currents in α7-nicotinic acetylcholine receptor, IC50=55±6 nM, and that (2S,6S)-hydroxynorketamine, (2R,6R)-hydroxynorketamine and (R,S)-norketamine also inhibited α7-nicotinic acetylcholine receptor function at concentrations ≤1 μM, while (R,S)-ketamine was inactive at these concentrations. The inhibitory effect of (R,S)-dehydronorketamine was voltage-independent and the compound did not competitively displace selective α7-nicotinic acetylcholine receptor ligands [125I]-α-bungarotoxin and [3H]-epibatidine indicating that (R,S)-dehydronorketamine is a negative allosteric modulator of the α7-nicotinic acetylcholine receptor. (R,S)-Ketamine and (R,S)-norketamine inhibited (S)-nicotine-induced whole-cell currents in cells expressing α3β4-nicotinic acetylcholine receptor, IC50 3.1 and 9.1 μM, respectively, while (R,S)-dehydronorketamine, (2S,6S)-hydroxynorketamine and (2R,6R)-hydroxynorketamine were weak inhibitors, IC50 >100 μM. The binding affinities of (R,S)-dehydronorketamine, (2S,6S)-hydroxynorketamine and (2R,6R)-hydroxynorketamine at the NMDA receptor were also determined using rat brain membranes and the selective NMDA receptor antagonist [3H]-MK-801. The calculated Ki values were 38.95 μM for (S)-dehydronorketamine, 21.19 μM for (2S,6S)-hydroxynorketamine and>100 μM for (2R,6R)-hydroxynorketamine. The results suggest that the inhibitory activity of ketamine metabolites at the α7-nicotinic acetylcholine receptor may contribute to the clinical effect of the drug. 相似文献
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