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??OBJECTIVE To develop a comprehensive analytical method based on UFLC-QTRAP-MS/MS for simultaneous determination of protopanaxadiol [ginsenoside Rb₁, Rc, Rb₂, Rd, F₂, 20(S)-Rg₃, 20(R)-Rg₃, CK], protopanaxatriol [ginsenoside Re, Rg₁, Rf, 20(S)-Rg₂, 20(S)-Rh₁, 20(R)-Rg₂, 20(R)-Rh₁, F₁] and oleanolic(ginsenoside Ro) in Ginseng Radix et Rhizoma and Ginseng Radix et Rhizoma Rubra. METHODS Under the optimized chromatographic conditions, good separation for seventeen target compounds was obtained on a Synergi^TM Hydro-RP 100?_ column(2.1 mm??100 mm, 2.5 ??m) at 40 ?? with 0.1% aqueous formic acid (A)/acetonitrile (B) as the mobile phase by gradient elution at a flow rate of 0.4 mL??min^-1. The target compounds were analyzed under multiple reaction monitoring (MRM) mode with an ESI source operated in negative ion mode, and principal component analysis (PCA) and hierarchical cluster analysis (HCA)were used for data processing. RESULTS The calibration curves of the 17 components had good linearity (r>0.999 0). The precision, repeatability and stability were all satisfying.The average recoveries of standard addition for the compounds were between 96.69% and 102.01%,and the relative standard deviations were less than 5%. The results of PCA and HCA showed that Ginseng Radix et Rhizoma and Ginseng Radix et Rhizoma Rubra were clearly distinguished.The main compositions with significant difference were ginsenoside 20(S)-Rg₃, 20(R)-Rg₃, 20(S)-Rh₁, 20(R)-Rh₁, and 20(R)-Rg₂. CONCLUSION The established method could provide a new technique for the comprehensive evaluation and quality control of Ginseng Radix et Rhizoma and Ginseng Radix et Rhizoma Rubra, at the same time, it would pave the way for discovering the material basis contributing to the different properties and efficacies of the two medicinal materials.     

基于人参皂苷和多糖含量的蒸制软支和硬支西洋参质量评价研究

目的 建立蒸西洋参的8个人参皂苷类成分以及多糖的含量测定方法。方法 采用高效液相色谱法(HPLC)测定自制蒸西洋参中8个人参皂苷类成分(人参皂苷Rg₁, Re, Rb₁, Rc, Rg₂, Rb₂, Rb₃, Rd)的含量,利用紫外-可见分光光度法(UV-Vis)对其总多糖的含量进行测定,并结合化学计量学(聚类分析、主成分分析、正交偏最小二乘判别分析等)的方法对所得结果进行分析。结果 来源于不同产地蒸西洋参的人参皂苷和多糖的含量有一定的差异,主要表现为软支西洋参蒸制后的各人参皂苷以及多糖的含量高于硬支,主成分分析(PCA)和偏最小二乘判别分析(OPLS-DA)结果也印证了这一结论。由以上研究可知,采用的蒸西洋参的方法较为稳定,所建立的基于8个人参皂苷类成分和多糖得率的含量测定方法可用于蒸西洋参的质量综合评价。结论 本研究为制定科学合理的蒸西洋参的加工方法和质量评价方法提供了依据。     

同仁堂红参与高丽红参品质的初步比较研究——人参皂苷和人参多糖的含量测定

目的：测定人参总皂苷,人参皂苷Rg₁,Re,Rb₁和人参多糖含量,比较同仁堂红参与高丽红参的质量。方法：建立大孔吸附树脂比色法测定人参总皂苷含量；采用二元梯度洗脱程序的高效液相色谱法测定人参皂苷Rg₁,Re,Rb₁的含量；优化试验条件,采用苯酚-硫酸显色方法测定人参多糖含量。结果：同仁堂红参中人参总皂苷含量不低于高丽红参中总皂苷的含量；人参皂苷Rg₁,Rb₁的含量与高丽红参中的含量相近,人参皂苷Re含量略低于高丽红参中的含量,而人参多糖含量则高于高丽红参中的含量。结论：同仁堂红参中人参皂苷含量不低于高丽红参中的含量且人参多糖含量高于高丽红参。建立的测定人参总皂苷、人参皂苷Rg₁,Re,Rb₁以及人参多糖含量的方法准确、快速、重复性好,可以作为人参质量定量评价的方法,初步比较不同来源的人参品质。     

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??OBJECTIVE To establish an HPLC method for simultaneous determination of ginsenoside Rg₁, Re, Rb₁ and jujuboside A, B in Renshen Jianpi Pellets (RSJPW). METHODS The determination was conducted on an Eclipse XDB C₁₈ column (4.6 mm??250 mm, 5 ??m) with the mobile phase of acetonitrile (A)-water (B) gradiently eluted at the following flow rates:0-90 min, 1.0 mL??min^-1; 90-130 min, 1.0-0.5 mL??min^-1; 130-140 min, 0.5 mL??min^-1. And the column temperature was maintained at 35 ??; the detection wavelength was set at 203 nm. RESULTS The calibration curves of ginsenoside Rg₁, Re, Rb₁ and jujuboside A, B were in good linearity over 0.32-2.24 ??g (r=0.998 2), 0.16-1.12 ??g (r=0.995 3), 0.32-2.24 ??g (r=0.999 6), 0.16-1.12 ??g (r=0.991 5), 0.08-0.56 ??g (r=0.999 6). The corresponding average recovery rates were 97.18%, 97.62%, 98.79%, 98.48%, 94.51%; the standard deviations were 1.10%, 0.98%, 0.34%, 1.09%, 1.88%, respectively. CONCLUSION The established HPLC method is accurate, reliable and reproducible, which can be used as a reference for the quality control of RSJPW.     

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??OBJECTIVE To establish a method for content determination of ginsenoside Rg₁, ginsenoside Rb₁, saikosaponin a, saikosaponin d, and saikosaponin B₂ in 70% ethanol elution effective fraction of Chaihu plus Longgu Muli decoction by HPLC-ELSD. METHODS A Diamonsil C₁₈ column(4.6 mm??250 mm, 5 ??m) was used as the stationary phase and the mobile phase consisted of acetonitrile and water. Gradient elution was carried out at the flow rate of 1.0 mL??min^-1. The column temperature was maitained at 30 ??. The ELSD detector was operated at 105 ?? with nebulizing gas at the optimum flow rate of 2.5 L??min^-1. RESULTS The average contents of ginsenoside Rg₁, ginsenoside Rb₁, saikosaponin a, saikosaponin d, and saikosaponin B₂ were 0.474%, 1.372%, 1.554%, 0.883%, and 2.073%, respectively. The calibration curves were linear in the ranges of 1.820-9.10, 1.810-9.050, 1.130-10.170, 0.420-2.100, and 3.125-15.625 ??g, respectively. The RSDs of precision, reproducibility and recovery were all less than 3.0%. CONCLUSION The method is rapid, simple, reliable and accurate, and has been successfully used to the quantification of five components in 70% ethanol elution effective fraction of Chaihu plus Longgu Muli decoction, which can provide a basis for the quality evaluation of Chaihu plus Longgu Muli decoction.     

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??OBJECTIVE To establish a measuring method for microdialysis probe recovery of ginsenoside Rg₁ and investigate the effects of flow rate, concentration and using times of probe on the recovery in vivo and in vitro. METHODS Dialysis method and retrodialysis method were used for the study. The concentration of ginsenoside Rg₁ in brain and blood dialysate was determined by LC-MS/MS and the probe recovery was calculated. RESULTS The recoveries of brain and blood microdialysis probes showed good stability within 10 h, with average values of 17.0% and 34.4% respectively for ginsenoside Rg₁ at 1.5 ??L??min^-1. Concentrations (50,200,500,1 000 ng??mL^-1) had no obvious effect on recovery. At the same concentration, the recovery of brain and blood probes for ginsenoside Rg₁ decreased with the increase of flow rate (0.5, 1.0, 1.5, 2.0, 3.0 ??L??min^-1) in vitro and in vivo. The dialysis recoveries of brain and blood probes in vitro were (40.6??4.3)%, (23.5??2.3)%, (17.7??0.8)%, (12.2??1.1)%, (8.8??0.6)% and (70.6??3.6)%, (46.0??2.1)%, (32.9??1.6)%, (25.6??0.7)%, (18.2??1.3)%, respectively. The recoveries of dialysis and retrodialysis in vitro were approximately equal, and the recovery detected by retrodialysis in vivo was similar with the in vitro results. Probe used for no more than 3 times still kept high transmittance by flushing with 2% heparin sodium and ultrapure water successively. CONCLUSION Retrodialysis method can be used to study brain and blood probe recovery in vivo, and microdialysis can be used for simutaneous pharmacokinetic studies of ginsenoside Rg₁ in intercelluar fluid and blood.     

HPLC-光敏二极管阵列检测法测定人参单体皂甙的研究

讨论了流动相为异丙醇－甲醇非水体系配合极性柱分离人参单体皂甙的情况。试验中选用了极性较强的NH2基键合相桂，以甲醇－异丙醇（62：38V／V）为流动相，选择二极管阵列检测器，UV204um处检测，分离了单体皂甙Re、Rg1、Rb1，方法操作简单、快速、重现性好，线性范围宽，检出限低，可用于人参及各种制剂的分析。     

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??OBJECTIVE To explore the effects of different bio-adhesive materials on in vitro adhesion and retention in artificial gastric acid fluid of Panax notoginseng saponins(PNS) bio-adhesive pellets.METHODS PNS bio-adhesive pellets were prepared with different bio-adhesive materials.The in vitro adhesion of PNS bio-adhesive pellets was determined by the tissue retention method, using HPLC method to determine the contents of PNS(including notoginseng saponins R₁, ginseng saponin Rg1 and ginseng saponin Rb₁) retained in the pellets after a certain period of time in artificial gastric acid fluid.RESULTS The contents of PNS retained in PNS bio-adhesive pellets prepared with chitosan and chitosan-carbomer after being placed in artificial gastric acid fluid for 2 h were the largest, which were (27.60??7.45)% and (19.80??3.55)% for R1, (27.01??5.49)% and (19.67??1.39)% for Rg₁ and (47.07??6.26)% and (51.08??7.44)% for Rb₁, respectively.For in vitro adhesion, HPMC and HPMC-carbomer combination was the best, followed by chitosan and chitosan-carbomer combination.CONCLUSION PNS bio-adhesive pellets prepared with chitosan and chitosan-carbomer combination bio-adhesive materials can protect PNS from degradation in artificial gastric acid fluid and have good adhesion property.     

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??OBJECITVE To establish an HPLC-MS/MS method for simultaneous determination of six active components in Dengyinnaotong capsules, ie, scutellarin, bilobalide, ginkgolide A, ginkgolide B, ginsenoside Rg₁ and notoginsenoside R₁. METHODS The chromatographic separation was carried out at 30 ?? on a Phenomenex Luna C₁₈ (4.6 mm??150 mm, 5 ??m) column eluted by gradient program. The flow rate was 0.3 mL??min^-1. The six compounds were separated within 10.0 min. RESULTS The regression curves for the six compounds showed good linearity in wide ranges. The recoveries were around from 94.8% to 108.5%. CONCLUSION The established method is accurate, reliable, specific and reproducible, which can be used for the quality control of Dengyinnaotong Capsules.     

HPLC-CAD法测定芪蛭通络胶囊中苷类成分的含量

目的 建立高效液相色谱-电喷雾检测器方法(HPLC-CAD)同时测定芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷的含量。方法 采用色谱柱为Waters XSclectHss T3-C₁₈(4. 6 mm×250 mm,5 μm),水(A)-乙腈(B)为流动相,梯度洗脱(0 min,15% B;0～10 min,15%~25%B;10～15 min,25%B~31%B;20～50 min,31%B),流速1 mL·min^{- 1},柱温25 ℃,进样量为20 μL。电喷雾检测器(CAD)雾化器温度为35 ℃,功能参数(power function,PF)为1.0。结果 芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷均具有良好的线性关系(r＞0.999 0),定量限(LOQ)分别为0.013和0.015 μg,精密度、重复性、24 h稳定性实验的相对标准偏差(RSD)值均小于3.0%,平均加样回收率分别为91.74%和100.09%。结论 本研究建立的HPLC-CAD法可同时对芪蛭通络胶囊中人参皂苷Rb₁和黄芪甲苷进行含量测定,为芪蛭通络胶囊的检测分析和质量控制提供了新的方法。