首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 160 毫秒
1.
目的:建立一测多评法(QAMS)同时测定血塞通片中三七皂苷R1、人参皂苷Rg1、人参皂苷 Re、人参皂苷Rb1、人参皂苷Rd 5种成分的含量。方法:采用高效液相法,使用Waters Symmetry Shield RP18色谱柱(4.6 mm×250 mm,5 μm),以乙腈-水溶液为流动相,梯度洗脱,流速1.3 mL·min-1, 柱温25 ℃,检测波长为203 nm。以人参皂苷Re为内标参照物,建立其与三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rd的相对校正因子(RCFs);通过一测多评法与外标法(ESM)结果的比较, 验证所建立方法的可行性和准确性。结果:5种皂苷在一定范围的浓度内呈良好的线性关系;三七皂苷 R1、人参皂苷Rg1、人参皂苷Rb1、人参皂苷Rd的相对校正因子分别为0.996、0.856、1.165、0.996;且在不同试验条件下重现性良好(RSD<3.0%)。结论:建立了血塞通片中5种成分的一测多评法,经方法学验证,该法可用于血塞通片中5种皂苷成分的含量测定。  相似文献   

2.
一测多评法测定复方人参片中的8种苷类成分   总被引:1,自引:1,他引:0  
目的 建立一测多评法(quantitative analysis single-marker,QAMS)测定复方人参片中8种苷类成分的含量。方法 采用Agilent XDB-C18色谱柱(4.6 mm×250 mm,5 μm),流动相水(A)-乙腈(B),梯度洗脱;体积流量1.0 mL·min-1;检测波长203 nm;柱温:25℃。以人参皂苷Rb1为内标,计算人参皂苷Rg1、人参皂苷Re、淫羊藿苷、人参皂苷Rc、人参皂苷Rb2、人参皂苷Rb3、人参皂苷Rd的相对校正因子,测定其含量。结果 8种成分在各自范围内线性关系良好(r ≥ 0.999 0),加样回收率为95.6%~104.4%,RSD为1.22%~2.73%,QAMS测定结果与外标法测定结果无显著性差异。结论 该法准确度、灵敏度高、专属性好、操作简单、重复性好。  相似文献   

3.
林庆新 《中国药师》2013,(10):1527-1528
摘 要 目的: 建立同时测定人参三七颗粒中人参皂苷Rg1、Re、Rb1和三七皂苷R1含量的方法。方法: 采用HPLC法,色谱柱为Sunfire C18(150 mm×4.6 mm,5 μm)分析柱,流动相以乙腈-水梯度洗脱;检测波长为203 nm;柱温30℃;流速1.0 ml·min-1。结果:人参皂苷Rg1,Re,Rb1和三七皂苷R1之间有较好的分离度,4种成分在线性范围内与峰面积之间线性关系良好,人参皂苷Rg1、Re、Rb1和三七皂苷R1加样回收率分别为99.83%,97.84%,98.43%,97.34%,RSD分别为2.08%,1.66%,1.73%和1.42%(n=5)。结论:本方法可同时测定人参三七颗粒中的人参皂苷Rg1,Re,Rb1和三七皂苷R1含量。  相似文献   

4.
目的 建立人参须药材质量标准。方法 采用经验、显微鉴别法对该药材性状、显微特征进行描述;按照中国药典2015年版四部通则相关方法,对药材水分、总灰分进行了测定;采用薄层色谱法,分别以人参对照药材和人参皂苷(Rb1、Re、Rf和Rg1)对照品为对照,对该药材的脂溶性成分及皂苷类成分进行定性鉴别;采用HPLC,以人参皂苷Re、Rg1、Rb1和Rb2为对照,采用Sepax BR-C18色谱柱(4.6 mm×250 mm,5 μm),乙腈-水为流动相,进行梯度洗脱,在203 nm波长下对各皂苷成分进行定量分析,建立该药材中皂苷类成分的含量测定方法。结果 该药材性状、显微、薄层鉴别方法具有较强的专属性,水分平均值为11.0%,总灰分平均值为4.6%,人参皂苷Re与Rg1总含量平均值为0.86%,Rb1含量平均值为0.54%,Rb2含量平均值为0.31%。结论 本研究依据实验结果和传统经验,同时结合了吉林省人参须药材的生产现状及药用企业的应用情况,可以作为人参须药材的质量标准。  相似文献   

5.
摘 要 目的:建立一测多评法(QAMS) 测定三七伤药片中6种活性成分含量。方法: 采用HPLC法,以Waters Sunfire ODS C18柱(250 mm×4.6 mm,5 μm)为色谱柱,流动相为乙腈 水,梯度洗脱,流速为1.0 ml·min-1,检测波长为可变波长(0 min,230 nm;10 min,283 nm;25 min,203 nm),柱温:30℃,进样量:10 μl。以柚皮苷为参照物,应用QAMS测定芍药苷、人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1和人参皂苷Re的相对较正因子并计算其含量,同时用外标法测定以上6种有效成分的含量,并将两种结果进行分析比校。结果: 一测多评法测得的芍药苷、人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1和人参皂苷Re 5种成分计算值与外标法测定值差异无统计学意义(P>0.05)。结论: QAMS法可用于三七伤药片6种指标性成分的含量测定,且方法简单、有效、结果准确。  相似文献   

6.
目的:建立三七总皂苷中三七皂苷R1,人参皂苷Rg1、Re、Rb1和Rd的一测多评含量测定方法(QAMS),并验证其准确性。方法:采用高效液相色谱法(HPLC),使用Welch PG C18色谱柱(250 mm×4.6 mm, 5μm),以乙腈-水为流动相,梯度洗脱,流速1.3 mL·min-1,柱温25℃,检测波长203 nm。分别采用标准曲线斜率法和浓度法测定,以人参皂苷Re为对照,分别计算其与三七皂苷R1,人参皂苷Rg1、Rb1和Rd的相对校正因子(RCFs),校正因子取2种方法的平均值,最终校正因子为3家省级以上食品药品监督检验研究院实验数据的平均值;采用一测多评法测定三七总皂苷中5个皂苷成分的含量。同时采用外标法测定三七总皂苷中5个皂苷成分的量,比较计算值与测定值之间的差异,验证一测多评法在测定中的准确性及可行性。结果:以人参皂苷Re为对照,三七皂苷R1,人参皂苷Rg1  相似文献   

7.
目的:建立活血止痛散和活血止痛胶囊中三七的专属性鉴别方法,并采用高分离度快速液相色谱-三重串联四极杆质谱(RRLC-QQQ/MS)对结果加以验证。方法:采用高效薄层色谱法研究三七与其混伪品人参、红参、三七茎叶的特征条带。以高效硅胶G薄层板为固定相,二氯甲烷-无水乙醇-水(70:45:6.5)展开,10%硫酸乙醇溶液显色,105℃加热至条带清晰。分别置紫外光灯(365 nm)和日光下检视。RRLC-QQQ/MS分析采用Agilent Rapid Resolution HT SB-C18(2.1 mm×100 mm,1.8 μm)色谱柱,以5 mmol·L-1醋酸铵溶液-乙腈为流动相梯度洗脱。离子化模式为ESI-,碎裂电压100 V。结果:三七可检出三七皂苷R1,未检出人参皂苷Rb3、人参皂苷Rf。人参和红参可检出人参皂苷Rb3和人参皂苷Rf,未检出三七皂苷R1。三七茎叶可检出人参皂苷Rb3,未检出三七皂苷R1或人参皂苷Rg1。以三七对照药材、三七皂苷R1(应检出)和人参皂苷Rb3(不得检出)为对照,可实现活血止痛制剂中三七的专属性鉴别和人参(红参)或三七茎叶的非法掺杂投料检查。6个厂家的93批样品均未发现人参、红参或三七茎叶冒充三七非法投料。RRLC-QQQ/MS与高效薄层分析结果一致。结论:该方法简便、快速、灵敏、准确,可为含三七中成药的质量控制提供参考。  相似文献   

8.
目的 研究大孔吸附树脂富集参血胶囊中人参皂苷Rb1的工艺条件。方法 采用HP1100高效液相色谱仪ZORBAX SB-C18柱(4.6 mm×250 mm,5 μm),紫外检测波长:203 nm,流动相:乙腈-水(30∶70)对人参皂苷Rb1进行测定。以树脂的比吸附量、比洗脱量及人参皂苷Rb1含量为指标,对树脂类型进行筛选,同时进行洗涤溶剂的选择,及应用L9(34)正交实验进行洗脱条件的研究,从而确定大孔吸附树脂纯化工艺参数。结果 人参皂苷Rb1在0.752~9.4 μg内呈现良好的线性关系,确定洗涤溶剂为0.5 mol·L-1 NaOH溶液,最佳洗脱条件:提取液上柱后静置12 h,用15倍60%的乙醇溶液,以流速1.0 mL·min-1进行洗脱。在此条件下,所得的人参皂苷Rb1含量较高。结论 该法简便、专属性强,可用于参血胶囊中人参皂苷Rb1的提取。  相似文献   

9.
目的 建立高效液相色谱一测多评(QAMS)法同时测定颈痛颗粒中三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、3''-羟基葛根素、葛根素、3''-甲氧基葛根素、洋川芎内酯A、藁本内酯、延胡索乙素、去氢紫堇碱、紫堇碱、羌活醇和异欧前胡素含量,并通过灰色关联度分析法对13种成分含量检测结果进行分析评价。方法 采用Shimadzu C18色谱柱;以乙腈-0.1%磷酸为流动相梯度洗脱;检测波长为203 nm(三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1)、280 nm(3''-羟基葛根素、葛根素、3''-甲氧基葛根素、洋川芎内酯A、藁本内酯、延胡索乙素、去氢紫堇碱和紫堇碱)和315 nm(羌活醇和异欧前胡素);采用外标法(ESM)测定13种成分的含量。以葛根素为内参物质,分别计算其与三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、3''-羟基葛根素、3''-甲氧基葛根素、洋川芎内酯A、藁本内酯、延胡索乙素、去氢紫堇碱、紫堇碱、羌活醇和异欧前胡素的相对校正因子(f),并计算上述12种成分的含量,比较ESM和QAMS法检测结果的差异,验证一测多评法的准确性和可行性。基于灰色关联度分析不同批次颈痛颗粒中13种成分QAMS法含量检测数据,对15批次颈痛颗粒质量进行综合评价。结果 三七皂苷R1、人参皂苷Rg1、人参皂苷Rb1、3''-羟基葛根素、葛根素、3''-甲氧基葛根素、洋川芎内酯A、藁本内酯、延胡索乙素、去氢紫堇碱、紫堇碱、羌活醇和异欧前胡素分别在各自范围内线性关系良好(r≥0.999 2),平均加样回收率(n=9)在96.86%~100.37%(RSD≤1.65%)。所建立的f耐用性良好,HPLC-QAMS法计算值和ESM实测值之间无明显差异。灰色关联度分析结果显示15批次颈痛颗粒相对关联度在0.332 4~0.600 4,表明颈痛颗粒批次间呈现一定质量差异。结论 QAMS多指标成分定量控制联合灰色关联度分析法操作便捷、结果准确,可用于颈痛颗粒的综合质量评价。  相似文献   

10.
目的 优化胃康颗粒中人参皂苷Rb1和黄芪甲苷的提取方法,并建立其含量测定方法。方法 以人参皂苷Rb1和黄芪甲苷的含量作为指标,采用单因素考察法对提取工艺进行优化;采用高效液相色谱-蒸发光散射法(HPLC-ELSD),XBridge®Shield RP18(4.6 mm×250 mm,5 μm)为色谱柱;乙腈-水(32:68)为流动相;柱温为30 ℃;漂移管温度为60 ℃,载气流量为1.7 SLM,建立测定胃康颗粒中人参皂苷Rb1和黄芪甲苷含量的方法。结果 当采用甲醇回流提取1.5 h,正丁醇提取5次,氨水洗涤2次时,人参皂苷Rb1和黄芪甲苷的提取含量较高;建立的HPLC-ELSD法测定人参皂苷Rb1和黄芪甲苷含量,线性关系良好(r > 0.9997),日内日间精密度均小于1%,加样回收率分别为95.65%和100.57%,稳定性和重复性的RSD均小于3%,含量分别为2.8630 mg/g和0.2576 mg/g,RSD分别为0.62%和1.51%。结论 优化了胃康颗粒中人参皂苷Rb1和黄芪甲苷的提取方法,建立了可靠、准确、重现性好的测定胃康颗粒中人参皂苷Rb1和黄芪甲苷含量的HPLC-ELSD方法。  相似文献   

11.
HPLC analysis of extracts of different parts of two six-year-old Panax ginseng (Ginseng & Tobacco Company, South Korea) plantation roots demonstrated the presence of seven detectable ginsenosides (Rb1, Rb2, Rc, Rd, Rf, Rg1, and Re). The total contents were 1.16 and 0.64% for main roots, 4.00 and 4.60% for rhizomes, 6.79, 4.38% for side roots (d = 0.4–0.5 cm), and 13.26 and 11.37 for fine roots (d = 0.1–0.15 cm). Four new ginseng callus lines were originated from side and fine roots. HPLC analysis of the qualitative and quantitative composition of the biomass after the first year of cultivation showed that all lines contained the full spectrum of ginsenosides (Rb1, Rb2, Rc, Rd, Rf, Rg1, and Re), the total content of which varied from 0.2 to 0.4%. HPLC monitoring of these callus lines over five years of cultivation demonstrated gradual disappearance of glycosides Rb2, Rc, Rd, and Rf from the ginsenoside spectrum. Loose calluses growing in medium containing 0.5 and 0.2 mg-liter 6-benzylaminopurine were used to start suspension cultures L-1 and L-2, respectively. HPLC analysis of the qualitative and quantitative composition of glycosides in suspension cultures showed that both lines contained only ginsenosides Rb1, Rg1, and Re, with a predominance of Re ginsenoside. __________ Translated from Khimiko-Farmatsevticheskii Zhurnal, Vol. 42, No. 1, pp. 33–38, January, 2008.  相似文献   

12.
人参皂苷水溶液热稳定性研究   总被引:4,自引:1,他引:3       下载免费PDF全文
目的 研究加热时间对人参皂苷水溶液的影响及受热后人参皂苷含量的变化情况。方法 红参须浓缩液加热不同时间,采用高效液相色谱法测定其人参皂苷Rg1、Re、Rb1、Rc和Rd的含量。结果 5种人参皂苷在加热6 h内,发生不同程度的降解反应,二醇类人参皂苷Rb1、Rc和Rd在加热2-3 h时,含量呈明显下降趋势,人参皂苷Rd降解速率最慢。三醇类人参皂苷Rg1和Re在加热3 h内含量快速下降,3 h后趋于平缓。结论 在常压受热条件下,人参皂苷水溶液主要成分人参皂苷Rg1、Re、Rb1、Rc和Rd的含量,随加热时间延长而不断下降,3 h后下降速率减缓。三醇类人参皂苷较二醇类对热更为敏感。  相似文献   

13.
This study systematically investigated the retention behavior of seven neutral ginsenosides Rg1, Re, Rf, Rb1, Rb2, Rc, Rd, and an acidic ginsenoside R0, the major pharmacologically active components of Radix Ginseng with RP-HPLC. The effects of solvent, pH value, ionic strength of the mobile phase, and column temperature were investigated using an octadecylsiloxane-bonded silica gel column. Based on the ginsenosides’ retention characteristics, the concentration of acetonitrile and the gradient of the mobile phase needed to maintain the baseline separation of the major neutral ginsenosides in Radix Ginseng were theoretically predicted. Furthermore, the ionic strength of mobile-phase necessary to achieve good resolution of the neutral ginsenosides and acidic ginsenosides was carefully investigated. According to the results of the quantitative analysis of ginsenosides in eight batches of ginseng samples from different sources, the developed HPLC technique may be a valuable tool for the quality assessment of Radix Ginseng.  相似文献   

14.
This study systematically investigated the retention behavior of seven neutral ginsenosides Rg1, Re, Rf, Rb1, Rb2, Rc, Rd, and an acidic ginsenoside R0, the major pharmacologically active components of Radix Ginseng with RP-HPLC. The effects of solvent, pH value, ionic strength of the mobile phase, and column temperature were investigated using an octadecylsiloxanebonded silica gel column. Based on the ginsenosides’ retention characteristics, the concentration of acetonitrile and the gradient of the mobile phase needed to maintain the baseline separation of the major neutral ginsenosides in Radix Ginseng were theoretically predicted. Furthermore, the ionic strength of mobile-phase necessary to achieve good resolution of the neutral ginsenosides and acidic ginsenosides was carefully investigated. According to the results of the quantitative analysis of ginsenosides in eight batches of ginseng samples from different sources, the developed HPLC technique may be a valuable tool for the quality assessment of Radix Ginseng. This article was retracted as it was printed by error in this issue of APR.  相似文献   

15.
闵春艳  游本刚  吴杨  郭青  狄恒建  顾炳仁 《中国药事》2017,31(11):1297-1303
目的:评价硫磺熏蒸对西洋参皂苷类成分的影响。方法:建立超高效液相色谱法,测定并比较分析硫磺熏蒸前后西洋参中人参皂苷Rg1、Re和Rb1的含量。结果:硫磺熏蒸后西洋参中人参皂苷Rg1、Re和Rb1总量仍符合《中国药典》规定;但当硫磺熏蒸致二氧化硫残留量大于400 mg·kg-1时,人参皂苷Re、Rb1的含量及人参皂苷Rg1、Re和Rb1三者的总量显著降低。当二氧化硫残留量不大于150 mg·kg-1时,人参皂苷Rg1、Re和Rb1的含量及其总量基本不受影响。结论:《中国药典》规定的西洋参二氧化硫残留量不得大于150 mg·kg-1有其科学合理性,硫磺过度熏蒸西洋参(二氧化硫残留量大于400mg·kg-1)对西洋参中皂苷类成分的含量有显著影响。  相似文献   

16.
目的 利用近红外光谱分析技术建立注射用益气复脉(冻干)主要原料红参醇提过程中3种单体皂苷——人参皂苷Rg1、Re和Rb1的定量模型,实现提取过程中关键指标的快速检测。方法 在线采集红参醇提过程的近红外光谱,以超高效液相色谱(UPLC)法测定提取过程药液中人参皂苷Rg1、Re和Rb1的量为参考值,采用偏最小二乘法建立光谱与测定值之间的定量校正模型,进而对提取过程进行在线分析。结果 人参皂苷Rg1和Re的建模波段均为9 403.7~7 498.3 cm-1和6 102~5 446.3 cm-1组合波段;人参皂苷Rb1的建模波段为5 774.1~5 446.3 cm-1。人参皂苷Rg1、Re、Rb1定量模型的交叉验证决定系数(R2)分别为99.40、99.44、99.41,交叉验证均方根误差分别为5.18、2.77、11.00。结论 所建立的3种单体皂苷定量模型预测性能良好,能够有效测定红参醇提过程中人参皂苷Rg1、Re和Rb1的量。  相似文献   

17.
Three new dammarane-type triterpene ginsenosides, together with six known ginsenosides, were isolated from the leaves of Panax ginseng C.A. Meyer. The new saponins were named as ginsenoside Rh11, ginsenoside Rh12, and ginsenoside Rh13. Their structures were elucidated as (20S)-3β,6α,12β,20-tetrahydroxydammara-25-ene-24-one 20-O-β-d-glucopyranoside (1), (20S)-3β,12β,20,24,25-pentahydroxydammarane 20-O-β-d-glucopyranoside (2), and (20S,23E)-3β,12β,20,25-tetrahydroxydammara-23-ene 20-O-β-d-glucopyranoside (3) on the basis of 1D and 2D NMR experiments and mass spectra. The known ginsenosides were identified as ginsenoside M7cd, ginsenoside Rg6, ginsenoside Rb3, gypenoside XVII, gypenoside IX, and 20-(E)-ginsenoside F4.  相似文献   

18.
The chemical characteristics for different parts of Panax notoginseng, including root, fibre root, rhizome, stem, leaf, flower and seed, were determined using high performance liquid chromatography-evaporative light scattering detection (HPLC-ELSD) and pressurized liquid extraction (PLE). Eight major saponins, namely notoginsenoside R1, ginsenosides Rg1, Re, Rb1, Rc, Rb2, Rb3 and Rd were also quantitatively compared among the different parts of P. notoginseng. The chromatograms showed that there was significant difference between underground (root, fibre root, rhizome) and aerial (leaf and flower) parts from P. notoginseng, though the similarities of entire chromatographic patterns among tested samples from underground (0.965 ± 0.029, n = 12) and aerial parts (0.987 ± 0.014, n = 5) were similar, respectively. Especially, no saponin was detected in the seed of P. notoginseng. Hierarchical clustering analysis based on eight investigated saponins or the ratios of contents for ginsenoside Rg1/Rb1 and ginsenoside Rb3/Rb1 showed that the samples from different parts of P. notoginseng were divided into three main clusters. One cluster was underground parts, which contained rich protopanaxatriol and protopanaxadiol types saponins. The leaf and flower were in the same cluster, which contained protopanaxadiol type saponins only. Especially, ginsenoside Rc, Rb2 and Rb3, rare in the underground parts, were rich in aerial parts of P. notoginseng. The stem of P. notoginseng was another cluster. Based on the cluster analysis, the chemical characteristics for different parts of P. notoginseng were revealed. They are composite cluster (underground parts), protopanaxadiol cluster (aerial parts) and interim (stem) cluster, which was the one between the two typical clusters, respectively. The result shows that chemical characteristics of underground parts and aerial parts from P. notoginseng are obviously different, which is helpful for pharmacological evaluation and quality control of P. notoginseng.  相似文献   

19.
A high-performance liquid chromatographic method with evaporative light scattering detection (HPLC–ELSD) has been developed to identify and quantify 19 ginsenosides (Rg1, Re, Rf, Rb1, Rc, Rb2, Rd, F4, Rg6, Rk3, Rh4, 20(S)-, 20(R)-Rg3, 20(S)-, 20(R)-Rs3, Rk1, Rg5, Rs4, and Rs5) in black ginseng (BG, Korean white ginseng that was subjected to nine cycles of steam treatment). Ultrasonication is employed for sample preparation, and the analysis is achieved on a Discovery C18 column using gradient elution of CH3CN–H2O–CH3COOH without buffer in 40 min. The method was validated by linearity (r2 ≥ 0.9994), precision (92.0–107.5%), intra- and inter-day accuracy (R.S.D. < 3.21%), and limit of detection (LOD ≤ 93 ng). The quantification method was applied to analyze the composition of ginsenosides in Korean white, red, and black ginsengs. During the preparatory process of BG, ginsenosides transform into constituents of low polarity by hydrolysis, isomerization, and dehydration at C-20, and hydrolysis also occurs at C-3 or C-6. The validated HPLC method is expected to provide the basis for the quality assessment of ginseng products.  相似文献   

20.
Fifty selected roots from a 7-year-old American ginseng (Panax quinquefolium L.) plant population grown in Denmark, with root weights varying from 191 to 490 g fresh weight (FW), were investigated for bioactive ginsenosides and polyacetylenes (PAs) in order to determine the correlation between the content of ginsenosides and PAs and root FW. PAs (falcarinol, panaxydol) and ginsenosides (Rb1, Rb2, Rb3, Rc, Rd, Re, Rg1) were extracted from roots by sequential extraction with ethyl acetate and 80% methanol, respectively, and quantified in extracts by reverse-phase high-performance liquid chromatography (HPLC) using photodiode array detection. Total concentrations of PAs and ginsenosides varied between 150 and 780 mg/kg FW and 5,920 and 15,660 mg/kg FW, respectively. No correlation existed between the content of ginsenosides and PAs and root FW or between the total concentration of ginsenosides and PAs. Strong significant correlation was found between total content of ginsenosides and ginsenoside Rb1 (r = 0.8190, P < 0.0001) and between total content of PAs and falcarinol (r = 0.9904, P < 0.0001). Based on the results of this study, it was concluded that it is possible to select large American ginseng roots for increased biomass production and concentration of bioactive ginsenosides and PAs without affecting the profile of bioactive compounds. Ginsenoside Rb1 and falcarinol were found to be important selection parameters for identifying superior genotypes with the highest content of bioactive compounds.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号