HPLC同时测定左归丸中的5种成分

目的 采用HPLC法同时测定左归丸中尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的含量.方法 采用依利特C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.2％磷酸溶液,梯度洗脱,流速1.3 mL· min-1,柱温为30℃,检测波长为224(尿囊素)、210(薯蓣皂苷元和梓醇)和330(麦角甾苷和吉奥诺苷B1)nm.结果 尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的线性范围分别为7.270～145.4μg·mL-1(r=0.9999)、5.150～103.0 μg·mL-1(r=0.9992)、5.730～114.6 μg·mL-1(r =0.9998)、6.740 ～134.8 μg·mL-1(r =0.9995)和5.100～102.0 μg·mL-1(r =0.9997);其平均加样回收率分别为98.37％、96.92％、99.11％、96.65％、98.31％,RSD分别为0.89％、1.28％、1.10％、0.57％、1.34％(n=6).结论 所用方法简便快捷、回收率好、重复性好,可用于左归丸中尿囊素、薯蓣皂苷元、梓醇、麦角甾苷和吉奥诺苷B1的含量测定.     

HPLC法同时测定杜仲补天素片中6种成分的含量

目的:建立同时测定杜仲补天素片中麦角甾苷、吉奥诺苷B_1、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸含量的方法。方法:采用高效液相色谱法。色谱柱为Kromasil C_(18),流动相为乙腈-0.2%磷酸溶液(梯度洗脱),流速为0.8 mL/min,检测波长为330 nm(麦角甾苷和吉奥诺苷B_1)、210 nm(去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸),柱温为35℃,进样量为10μL。结果:麦角甾苷、吉奥诺苷B_1、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸检测质量浓度线性范围分别为3.71~74.20μg/mL(r=0.9999)、4.35~87.00μg/mL(r=0.999 5)、3.86~77.20μg/mL(r=0.999 9)、5.05~101.00μg/mL(r=0.999 1)、4.20~84.00μg/mL(r=0.9997)、4.73~87.40μg/mL(r=0.999 6);定量限分别为0.322、0.187、0.105、0.381、0.214、0.452μg/mL,检测限分别为0.108、0.059、0.032、0.131、0.072、0.149μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为96.20%~99.53%(RSD=1.23%,n=6)、96.99%~100.67%(RSD=1.47%,n=6)、96.64%~100.08%(RSD=1.28%,n=6)、97.47%~100.59%(RSD=1.18%,n=6)、97.97%~100.83%(RSD=1.25%,n=6)、96.81%~99.61%(RSD=1.09%,n=6)。结论:该方法操作简便、快速、准确,可用于杜仲补天素片中麦角甾苷、吉奥诺苷B_1、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸含量的同时测定。     

商茯苓中三萜类成分的质量控制

目的 控制商茯苓的质量。方法 采用TLC法鉴别商茯苓药材中的三萜类化合物,HPLC法同时测定去氢土莫酸、猪苓酸C、去氢茯苓酸、茯苓酸等的含量。结果 13.8～110.4μg·mL^-1去氢土莫酸、4.28～34.24μg·mL^-1猪苓酸C、6.24～49.92μg·mL^-1去氢茯苓酸、14.4～115.2μg·mL^-1茯苓酸与峰面积呈良好的线性关系,r分别为0.9999、0.9998、0.9999、0.9999。平均加样回收率分别为99.57%、98.83%、101.36%、100.29%,RSD分别为2.30%、2.56%、2.27%、1.82%。结论 所用方法的专属性较强,能准确进行定性和定量鉴别,可用于商茯苓药材的质量控制。     

波长转换RP-HPLC法同时测定茯苓不同部位中5种三萜酸含量

建立同时测定茯苓不同部位中去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸和茯苓酸含量的方法。采用紫外-波长转换检测的RP-HPLC法: 色谱柱为Kromasil C₁₈柱 (250 mm × 4.6 mm, 5 μm); 流动相为乙腈 (A)-0.05%磷酸水溶液 (B) 系统, 梯度洗脱 (0～5 min, 60%A～64%A; 5～35 min, 64%A～65%A; 35～35.01 min, 65% A～73% A; 35.01～53 min, 73% A); 流速为1.0 mL·min⁻¹; 检测波长为0～48 min, 241 nm (去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸), 48～55 min, 210 nm (茯苓酸)。去氢土莫酸、猪苓酸C、3-表去氢土莫酸、去氢茯苓酸和茯苓酸分别在30.5～610.0 μg·mL⁻¹ (r = 0.999 6)、12.66～253.2 μg·mL⁻¹ (r = 0.999 5)、2.99～59.7 μg·mL⁻¹ (r = 0.999 7)、6.13～122.5 μg·mL⁻¹ (r = 0.999 5)、11.3～226.0 μg·mL⁻¹ (r = 0.999 5) 内浓度与峰面积呈良好的线性关系; 方法回收率分别为98.5% (RSD = 1.9%)、99.4% (RSD = 1.7%)、97.9% (RSD = 1.2%)、96.7% (RSD = 2.5%) 和97.9% (RSD = 2.3%)。结果表明, 本方法简便、准确、重现性好, 为茯苓药材的质量控制提供了依据。     

HPLC法测定威喜丸中猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸

目的建立HPLC波长切换法同时测定威喜丸中猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸的方法。方法采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–0.05%磷酸溶液,梯度洗脱;0～24.0 min在248 nm波长下检测猪苓酮B和猪苓酮A,24.0～50.0 min在210 nm波长下检测去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸;体积流量1.0m L/min;柱温30℃;进样量为10μL。结果猪苓酮B、猪苓酮A、去氢土莫酸、猪苓酸C、去氢茯苓酸和茯苓酸分别在5.79～115.80、1.66～33.20、3.28～65.60、7.07～141.40、1.46～29.20、0.88～17.60μg/mL与峰面积线性关系良好;平均加样回收率分别为98.75%、97.60%、98.23%、99.49%、97.10%、96.81%,RSD值分别为0.75%、1.66%、1.44%、0.90%、1.15%、1.38%。结论本方法简便、准确、重复性好,为威喜丸的质量控制提供了实验依据。     

RP-HPLC法同时测定五加参口服液中10个成分的含量

目的:建立同时测定五加参口服液中紫丁香苷、刺五加苷E、异嗪皮啶、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁、去氢土莫酸、去氢茯苓酸、茯苓酸和松苓新酸10个成分的含量测定方法。方法:采用反相高效液相色谱法,色谱柱为SHIMADZU-GL Wondasil C₁₈-WR色谱柱(250 mm×4.6 mm, 5μm),以乙腈-0.3%磷酸水溶液为流动相进行梯度洗脱,流速为1.0 mL·min^-1,检测波长为203 nm,柱温为35℃。结果:紫丁香苷、刺五加苷E、异嗪皮啶、人参皂苷Rg₁、人参皂苷Re、人参皂苷Rb₁、去氢土莫酸、去氢茯苓酸、茯苓酸和松苓新酸检测质量浓度的线性范围分别为10.74～80.55、7.04～52.8、2.932～21.99、2.232～16.74、5.84～43.8、10.42～78.15、2.544～19.08、1.9～14.25、3.272～24.54、0.642～4.815μg·mL^-1(r=0.999 3...     

HPLC波长切换法同时测定琥珀多寐丸中6个成分的含量

目的建立同时测定琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸含量的方法。方法采用波长切换检测的高效液相色谱法,色谱柱采用依利特C_(18)色谱柱,流动相为乙腈(A)-体积分数为0.1%的磷酸溶液(B)系统,进行梯度洗脱;0~36 min检测波长为320 nm(检测远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖),36~75 min检测波长为210 nm(检测细叶远志皂苷、远志皂苷B、去氢土莫酸、茯苓酸);流速为1.3 mL·min~(-1);柱温为30℃。结果在优化的色谱条件下,远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸分别在6.46~129.20 mg·L~(-1)(r=0.999 2)、6.13~122.60 mg·L~(-1)(r=0.999 5)、13.17~263.40 mg·L~(-1)(r=0.999 9)、14.15~283.00 mg·L~(-1)(r=0.999 6)、5.35~107.00 mg·L~(-1)(r=0.999 7)、4.50~90.00 mg·L~(-1)(r=0.999 3)内浓度与峰面积呈良好的线性关系;6种成分的平均加样回收率(n=6)分别为97.69%、96.87%、100.04%、97.74%、97.67%、99.16%,RSD分别为1.35%、0.96%、0.59%、0.93%、1.02%、1.10%。结论该检测方法可用于琥珀多寐丸中远志(口山)酮Ⅲ、3,6'-二芥子酰基蔗糖、细叶远志皂苷、远志皂苷B、去氢土莫酸和茯苓酸的含量分析。     

HPLC法测定参苓健体粉中去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ和白术内酯Ⅰ

目的建立梯度洗脱联合波长切换高效液相色谱(HPLC)法对参苓健体粉中去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯Ⅲ和白术内酯Ⅰ同时进行测定。方法采用Venusil MP C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–0.05%磷酸溶液,梯度洗脱;检测波长:210 nm(0~19 min,检测去氢土莫酸、去氢茯苓酸和茯苓酸)、220 nm(19~35 min,检测白术内酯Ⅲ和白术内酯Ⅰ);体积流量:0.8 m L/min;柱温:30℃;进样量为10μL。结果去氢土莫酸、去氢茯苓酸、茯苓酸、白术内酯III、白术内酯I质量浓度分别在4.62~92.40μg/m L(r=0.999 7)、3.80~76.00μg/m L(r=0.999 9)、5.76~115.20μg/m L(r=0.999 9)、3.95~79.00μg/m L(r=0.999 8)、5.05~101.00μg/m L(r=0.999 6)与峰面积关系良好;回收率分别为99.24%、97.75%、98.66%、98.49%、99.10%,RSD值分别为1.23%、1.79%、1.66%、0.80%、1.25%。结论建立的方法操作简便、结果可靠,可用于参苓健体粉的质量控制。     

RP-HPLC法测定中药茯苓皮中茯苓酸A和3-表去氢土莫酸的含量

目的：建立一种可用于评价茯苓皮药材质量的含量测定方法。方法：采用Dikma Dimonsal C18色谱柱（250mm×4.6mm,5μm）,以0.1％甲酸水溶液和乙腈为流动相,流速：1.0mL·min^-1,检测波长：243nm,柱温：25℃,用梯度洗脱法同时测定茯苓皮药材中茯苓酸A和3-表去氢土莫酸的含量。结果：测得茯苓酸A和3.表去氢土莫酸的线性范围分别为0.073-0.292g·L^-1（r=0.9997）和0.027—0.135g·L^-1（r=0.9999）;加样回收率分别为102.63％和98.88％。结论：该法能快速、准确地测定茯苓皮中两个活性成分的含量,为茯苓皮的质量控制提供了一个较好的检测方法。     

HPLC法测定八味肾气丸中去氢土莫酸、茯苓酸、梓醇和桃叶珊瑚苷

目的建立同时测定八味肾气丸中去氢土莫酸、茯苓酸、梓醇、桃叶珊瑚苷4个成分的高效液相色谱测定方法.方法采用Hypersil C18色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈–0.1%磷酸溶液,梯度洗脱;检测波长:0~18 min, 241 nm(去氢土莫酸);18~50 min,210 nm(茯苓酸、梓醇和桃叶珊瑚苷);体积流量为1.0 mL/min;柱温25℃;进样量20 μL.结果去氢土莫酸、茯苓酸、梓醇和桃叶珊瑚苷分别在3.35~67.00μg/mL、3.50~70.00μg/mL、3.07~61.40μg/mL、3.25~65.00μg/mL线性良好,r值均大于0.999 0,平均回收率分别为96.72%、97.87%、98.21%、98.09%,RSD值分别为1.08%、0.95%、0.64%、1.22%(n=6).结论 该方法简便,结果准确,可用于八味肾气丸中去氢土莫酸、茯苓酸、梓醇、桃叶珊瑚苷的质量控制.     

Comparison of the choleretic properties of bile acids

The choleretic properties of cholic, chenodeoxycholic, and deoxycholic acid and their taurine and glycine conjugates were compared to their ability to form micelles. It has previously been concluded that deoxycholate has the lowest critical micellar concentration; chenodeoxycholate is slightly higher and cholic is much higher. Conjugation with glycine and taurine has little or no effect on the critical micelle concentration. Since the choleretic properties of bile salts are thought to be directly proportional to their osmotic activities, one might suspect that deoxycholic acid would be the least choleretic, chenodeoxycholic slightly more choleretic and cholic much more choleretic, with little difference between the conjugated and unconjugated forms. However, in the present study, cholic, chenodeoxycholic and taurocholic acid produced similar increases in bile flow (450–700 μl/kg) after an equimolar dose (55 μM/kg). Except for the conjugation of deoxycholic acid with taurine, conjugation of these bile acids with glycine or taurine always decreased the choleretic properties of the bile acids. Therefore, it has been concluded that there is not a good correlation between the in vitro osmotic properties of bile acids and their ability to increase bile flow.     

抗癌活性成分满五酸等三个化合物的分离和鉴定

从产于四川宜宾翼梗五味子果实中,分得抗癌活性成分满五酸(1),同时分得schizandronic acid(2)和cuparenic acid(3),结构由与标准化合物比较光谱数据和物理常数而确证。     

Pomegranate (<Emphasis Type="Italic">Punica granatum</Emphasis>) pure chemicals show possible synergistic inhibition of human PC-3 prostate cancer cell invasion across Matrigel™

Summary Four pure chemicals, ellagic acid (E), caffeic acid (C), luteolin (L) and punicic acid (P), all important components of the aqueous compartments or oily compartment of pomegranate fruit (Punica granatum), and each belonging to different representative chemical classes and showing known anticancer activities, were tested as potential inhibitors of in vitro invasion of human PC-3 prostate cancer cells in an assay employing Matrigel™ artificial membranes. All compounds significantly inhibited invasion when employed individually. When C, P, and L were equally combined at the same gross dosage (4 μ g/ml) as when the compounds were tested individually, a supradditive inhibition of invasion was observed, measured by the Kruskal-Wallis non-parametric test.An erratum to this article can be found at     

HPLC法测定熊去氧胆酸片有关物质的含量

[摘要]目的：建立高效液相色谱法测定熊去氧胆酸片有关物质含量的方法。方法：用十八烷基硅烷键合硅胶为填充剂，以磷酸盐缓冲液（pH3.0）-甲醇-乙腈（35:37:28）为流动相，示差折光检测器测定。结果：在选定的色谱条件下，各成分可达到很好的分离，7-酮基胆石酸、胆酸、鹅去氧胆酸、胆石酸分别在0.05~2.00，0.05~2.00，0.05~2.00，0.10~2.00mg·mL-1的范围内线性关系良好(r>0.9989)；精密度、稳定性试验的RSD均不大于0.5%；回收率分别为100.1%、99.8%、100.7%和101.9%（n=9,RSD<1.4%）。7-酮基胆石酸、胆酸、鹅去氧胆酸、胆石酸定量限分别为3.0、2.5、7.0、20μg·mL-1，检测限分别为0.8、0.7、2.0、3.5μg·mL-1。测定供试品两批，供试品一7-酮基胆石酸检出量为0.03%，胆酸和胆石酸均未检出，鹅去氧胆酸检出量为0.66%；供试品二7-酮基胆石酸、鹅去氧胆酸检出量均为0.10%，胆酸和胆石酸均未检出。结论：该方法灵敏度高，专属性强，适于测定熊去氧胆酸片中有关物质的含量。     

Antitumor triterpenes from medicinal plants

Thirteen kinds of naturally occurring or derivatised triterpenes, reported to have an antitumoral property, were reinvestigated on the basis of their direct cytotoxicity or the inhibitory activity on cell growth against five kinds of cultured human tumor cells,i. e., A-549, SK-OV-3, SK-MEL-2, XF498 and HCT15,in vitro. Ursonic acidIII, betulinic acidVIII, betulonic acidX and glycyrrhetinic acidXI were exhibited a marked inhibition on cell growth.     

HPLC同时测定升麻中三个酚酸类成分的含量

目的建立快速测定升麻中咖啡酸、阿魏酸及异阿魏酸含量的HPLC方法。方法色谱柱为C18柱(4.6 mm×250 mm,5μm);流动相:乙腈-0.01%磷酸梯度洗脱;柱温:30℃;检测波长:320 nm;流速:1.0 ml/min。结果咖啡酸、阿魏酸、异阿魏酸分别在5.78~115.6μg/ml(r=0.9998,n=6),4.03~80.60μg/ml(r=1,n=6),16.45~329.00μg/ml(r=1,n=6)范围内线性关系良好,回收率在97.6%~101.5%。结论建立的方法准确可靠,可以用于测定升麻中咖啡酸、阿魏酸、异阿魏酸的含量。     

HPLC测定L-天门冬氨酸中的有关物质

目的建立L-天门冬氨酸中羟基丁二酸、丁二酸和富马酸等有关物质的检查方法。方法采用HPLC法,使用AQ C18色谱柱,0.01 mol.L-1的磷酸二氢钾水溶液(磷酸调pH3)为流动相,检测波长200 nm。结果主成分和杂质可完全分离。结论建立的方法灵敏、专属,可用于L-天门冬氨酸中有关物质的测定。     

Oral antipyretic therapy: Evaluation of the N-aryl-anthranilic acid derivatives mefenamic acid,tolfenamic acid and flufenamic acid

Summary The antipyretic activity of three N-aryl-anthranilic acid derivatives, mefenamic acid, tolfenamic acid and flufenamic acid, was compared and their optimal antipyretic dose determined in a trial in 87 children (aged 5 months to 15 years), who suffered from infections and fever exceeding 38.5°C. Tolfenamic acid proved to be the most potent antipyretic agent of the three drugs; it was eight times more powerful than mefenamic acid and three times more powerful than flufenamic acid. The optimal antipyretic doses were: mefenamic acid 4 mg/kg, tolfenamic acid 0.5 mg/kg and flufenamic acid 1.5 mg/kg. It is evident that the antipyretic activity of these anthranilic acid derivatives is even greater than their antirheumatic effect, the difference being most noticeable in the case of tolfenamic acid.