RP-HPLC测定半枝莲药材中4种主要黄酮类成分的含量

 目的建立测定半枝莲药材中野黄芩苷、野黄芩素、木犀草素和芹菜素含量的HPLC分析方法。方法采用C₁₈柱,测定野黄芩苷以甲醇-0.1%醋酸水溶液(40∶60)为流动相;测定野黄芩素、木犀草素和芹菜素以乙腈-0.1%醋酸水溶液为流动相,梯度洗脱(0→40min,乙腈15%→60%)。流速为1.0mL·min^-1,检测波长为335nm。结果野黄芩苷、野黄芩素、木犀草素和芹菜素分别在0.0124～0.992μg,0.006675～0.6675μg,0.00484～0.484μg和0.006875～0.6875μg内呈良好的线性关系。所测10份半枝莲药材中,野黄芩苷、野黄芩素、木犀草素和芹菜素的含量范围分别为0.147%～0.592%,0.028%～0.296%,0.007%～0.084%和0.011%～0.217%。结论本方法简便可行,适用于半枝莲药材中4种黄酮类成分的含量测定。     

HPLC法测定清肝散结颗粒中黄芩苷、汉黄芩苷、野黄芩苷、黄芩素及汉黄芩素

目的对清肝散结颗粒(猫人参、石见穿、白花蛇舌草、半枝莲及黄芩等)中所含的黄酮类化学成分黄芩苷、汉黄芩苷、野黄芩苷、黄芩素及汉黄芩素同时进行测定,建立制剂质量控制方法。方法采用高效液相色谱法,Waters Xterra Rp-C18色谱柱(3.0 mm×100 mm,3.5μm),流动相为乙腈(A)与0.1%甲酸水溶液(B),梯度洗脱,体积流量0.4 mL/min,柱温20℃,紫外检测波长为275 nm,进样量5μL,运行时间60 min。结果 5个待测化合物与周围干扰峰达到基线分离,线性范围分别为黄芩苷4.604⁴60.4μg/mL(r=0.999 9);汉黄芩苷0.770 4460.4μg/mL(r=0.999 9);汉黄芩苷0.770 4⁷7.04μg/mL(r=0.999 6);野黄芩苷0.415 777.04μg/mL(r=0.999 6);野黄芩苷0.415 7⁴1.57μg/mL(r=0.999 8);黄芩素0.845 641.57μg/mL(r=0.999 8);黄芩素0.845 6⁸4.56μg/mL(r=0.999 9);汉黄芩素0.799 284.56μg/mL(r=0.999 9);汉黄芩素0.799 2⁷9.92μg/mL(r=0.999 7),日内/日间精密度均小于3%(n=3),平均回收率在97%79.92μg/mL(r=0.999 7),日内/日间精密度均小于3%(n=3),平均回收率在97%¹02%之间(n=6)。清肝散结颗粒中黄芩苷、汉黄芩苷、野黄芩苷、黄芩素及汉黄芩素的含有量分别为3.798、0.829 9、0.180 5、0.158 9、0.0726 mg/g。结论该法简便、快捷、结果准确、重复性好、实用性强,可用于清肝散结颗粒中的质量控制。     

HPLC同时测定清热解毒胶囊中6种成分的含量

目的:建立HPLC测定清热解毒胶囊中绿原酸、栀子苷、木犀草苷、黄芩苷、连翘苷和汉黄芩素含量的方法。方法:采用Eclipse XDB色谱柱(4.6 mm×150 mm,5μm),流动相乙腈-0.4%磷酸溶液,梯度洗脱,流速0.80 m L·min-1,检测波长275nm。绿原酸、栀子苷、木犀草苷、黄芩苷、连翘苷和汉黄芩素与其相邻质谱峰能完全分离。结果:绿原酸、栀子苷、木犀草苷、黄芩苷、连翘苷和汉黄芩素的线性范围分别为7.83~313 mg·L-1(r=0.999 9),4.30~132 mg·L-1(r=0.999 8),0.836~33.5 mg·L-1(r=0.999 7),4.36~349 mg·L-1(r=1.000 0),0.731~58.4 mg·L-1(r=0.999 7),0.314~12.6 mg·L-1(r=0.999 7)。方法回收率均不低于98%。结论:该方法简便、准确、重复性好,能排除其他成分的干扰,可用于该制剂的质量控制的评价。     

半枝莲化学成分及抑制血管生成活性的研究

 目的 研究半枝莲的化学成分及其抑制血管生成活性。方法 采用硅胶柱色谱、sephadex LH-20凝胶柱色谱分离纯化化合物,运用理化反应和波谱分析鉴定化合物的结构。采用斑马鱼抑制血管生成模型测试化合物的活性。结果 从半枝莲体积分数75%乙醇提取物中的乙酸乙酯萃取部分中分离得到了9个化合物,分别为：汉黄芩素,4′-羟基汉黄芩素,芹菜素,黄芩素,柚皮素,木樨草素,异鼠李素,野黄芩苷,黄芩苷,其中异鼠李素有明显的抑制血管生成活性。结论 抑制血管生成是半枝莲抗肿瘤作用的途径之一。     

HPLC法同时测定15个产地浮萍中4种黄酮类成分

目的建立HPLC法同时测定15个产地浮萍Spirodela polyrriza(L.)Schleid.中4种黄酮类成分(荭草苷、牡荆苷、木犀草素、芹菜素)的含有量。方法分析采用Waters XBridge C18色谱柱(4.6 mm×150 mm,5μm);流动相甲醇-0.5%磷酸水溶液,梯度洗脱;体积流量1.0 m L/min;柱温25℃;检测波长350 nm。结果荭草苷在0.228 0~5.700 0μg(R~2=0.999 7)、牡荆苷在0.086 4~5.400 0μg(R~2=0.999 8)、木犀草素在0.132 0~5.500 0μg(R~2=0.999 8)、芹菜素在0.026 4~6.600 0μg(R~2=0.999 9)范围内具有良好的线性关系,平均加样回收率为100.31%~104.58%,其含有量依次为荭草苷牡荆苷木犀草素芹菜素。结论不同产地浮萍中荭草苷和牡荆苷的含有量有明显差异,而木犀草素和芹菜素比较稳定。     

RRLC法同时测定蒲地蓝消炎胶囊中绿原酸、野黄芩苷、黄芩苷和黄芩素的含量

目的 建立高分离度快速液相色谱(RRLC)法同时测定蒲地蓝消炎胶囊中绿原酸、野黄芩苷、黄芩苷和黄芩素的方法。方法 采用ZORBAX SB-C18柱(150 mm × 4.6 mm,1.8 μm),0.4 %磷酸水溶液-乙腈为流动相的梯度洗脱模式分离各测定组分,采用可变波长的方式在最大吸收波长处测定相应组分的峰面积并计算样品含量。结果 绿原酸、野黄芩苷、黄芩苷和黄芩素分别在0.004330~0.4330 μg(r = 0.9999)、0.01740~1.740 μg(r = 0.9998)、0.005860~0.5860 μg(r = 0.9998)及0.006700~0.6700 μg(r = 0.9999)范围内具有良好的线性关系;且平均加样回收率和RSD分别为101.0 %,2.0 %;103.1 %,1.7 %;100.6 %,0.6 %;102.0 %,0.7 %(n = 6);重复性试验,4个成分含量的RSD均小于2.0 %(n = 6)。结论 所建立的方法简便、快速、准确,具有良好的重复性和稳定性,可用于蒲地蓝消炎胶囊的质量控制。     

HPLC同时测定复方金银花颗粒中绿原酸、连翘苷、黄芩苷、汉黄芩素、芹菜素的含量

目的:建立同时测定复方金银花颗粒中5种化学成分(绿原酸、连翘苷、黄芩苷、汉黄芩素、芹菜素)的高效液相色谱法。方法:采用Agilent-Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm)。以甲醇(A)-0.2%磷酸溶液(B)为流动相进行梯度洗脱(0~10 min,25%~53%A;10~16 min,53%~78%A),检测波长278 nm,流速1 mL·min-1,进样量为20μL,柱温25℃。结果:绿原酸、连翘苷、黄芩苷、汉黄芩素、芹菜素5种成分在25 min内基本分离。峰面积(Y)对进样量(X)的标准曲线分别为绿原酸Y=2 350.4X-137.27,r=0.999 6;连翘苷Y=1 161.7X+18.474,r=0.999 6;黄芩苷Y=3 204.2X-423.45,r=0.998 8;汉黄芩苷Y=4 792.7X-93.15,r=0.998 5;芹菜素Y=1 434.1X-8.4132,r=0.999 3;加样回收率分别为:绿原酸99.47%(RSD 0.8%);连翘苷98.26%(RSD 0.9%);黄芩苷100.4%(RSD 1.9%);汉黄芩素99.29%(RSD 1.1%);芹菜素98.79%(RSD 1.1%)。结论:该方法操作简便,重复性好,分离效果好,可以作为复方金银花颗粒的质量控制。     

UFLC法同时测定黄芩中4种活性成分的含量

目的:建立超快速液相色谱法同时测定黄芩中黄芩苷、汉黄芩苷、黄芩素和汉黄芩素的含量。方法:采用Shim-Pack XR-ODS柱(75 mm×3.0 mm,2.2μm);流动相为0.1%磷酸水溶液(A)-乙腈(B)梯度洗脱(0~11 min,35%~41%B;11~12 min,41%~35%B),平衡时间2 min;流速为0.4 m L·min-1;检测波长为275nm;柱温为30℃。结果:黄芩苷、汉黄芩苷、黄芩素和汉黄芩素分别在20~200μg·mL~(-1)(r=0.999 6)、4.0~40μg·mL~(-1)(r=0.999 5)、0.1~1.0μg·mL~(-1)(r=0.999 3)和0.4~4.0μg·mL~(-1)(r=0.999 6)浓度范围内与峰面积呈良好的线性关系;平均回收率(n=9)分别为99.2%,98.2%,98.7%和99.1%。结论:该方法结果准确、操作简便、具有良好的重现性和稳定性,可用于黄芩药材的质量控制。     

HPLC 法同时测定蒺藜茎叶中3 个黄酮醇苷的含量

目的：建立HPLC法同时测定蒺藜茎叶中含量较高的3个黄酮醇苷类化合物的含量。方法：色谱柱：Thermo Syncronis C18（250 mm×4.6 mm,5 μm）;流动相：水（A）-乙腈（B）,梯度洗脱,0~30 min,8%~27% B;检测波长：254 nm;柱温：40℃;流速：1.0 mL·min-1;进样量：20 μL。结果：异鼠李素-3-O-β-D-龙胆双糖基-7-O-β-D-葡萄糖苷、槲皮素-3-O-β-D-龙胆双糖苷、异鼠李素-3-O-β-D-龙胆双糖苷分别在0.011 2~0.280 0 μg（r=0.999 6）、0.064 8~2.592 0 μg（r=0.999 8）、0.018 4~0.460 0 μg（r=0.999 8）范围内线性关系良好;平均加样回收率（n=9）分别为100.15%（RSD=1.32%）、100.02%（RSD=1.14%）、99.77%（RSD=1.16%）。结论：该方法简便、快速、准确、灵敏,为蒺藜或其制剂的质量控制和综合评价提供参考。     

HPLC同时测定黄栀花口服液中绿原酸、栀子苷、黄芩苷、黄芩素和汉黄芩素的含量

目的:建立同时测定黄栀花口服液(金银花、栀子、黄芩等)中绿原酸、栀子苷、黄芩苷、黄芩素与汉黄芩素含量的方法。方法:采用HPLC法,Agilent SB-C18色谱柱(4.6 mm×250 mm,5μm);流动相乙腈(A)-0.1%的磷酸溶液(B),梯度洗脱,流速1.0 m L·min-1;检测波长(0~13 min,327 nm;13~15 min,238 nm;15~45 min,280nm)。结果:根据回归方程,5种成分线性范围分别为绿原酸4.096×10-3~1.228 8×10-1μg(r=0.999 3);栀子苷4.204×10-3~1.261 2×10-1μg(r=0.999 9);黄芩苷0.117 5~3.525μg(r=0.999 9);黄芩素4.152×10-3~1.245 6×10-1μg(r=0.999 9);汉黄芩素4.256×10-4~1.276 8×10-2μg(r=0.999 4);平均回收率分别为绿原酸99.31%,RSD 0.8%,栀子苷99.62%,RSD 0.5%,黄芩苷99.94%,RSD1.3%,黄芩素99.64%,RSD 0.8%,汉黄芩素100.1%,RSD 1.2%。结论:该方法操作简便、准确、重复性好,可用于黄栀花口服液的质量控制。     

微波消解-电感耦合等离子体质谱法测定脉络宁注射液中25种矿物质元素

目的建立微波消解-电感耦合等离子体质谱(ICP-MS)直接稀释测定脉络宁注射液中25种矿物质元素(Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V、As、Cd和Hg)的方法。方法分别对微波消解条件和测试条件进行考察;样品经微波消解后,采用电感耦合质谱仪测定25种矿物质元素,并对测定方法学进行考察。结果确定最佳消解条件为3步缓慢升温:400 W 80℃升温10 min,保留5 min;600 W 120℃升温10 min,保留5 min;900 W 200℃升温20 min,保留20 min;25种矿物质元素在各自的线性范围内线性关系良好,r≥0.999 6,精密度、稳定性和重复性试验的RSD均符合定量分析要求;加标回收率为94.7%~106.1%,RSD在0.34%~2.79%。脉络宁注射液中检测出Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V,未检出As、Cd和Hg。结论该方法简便、迅速、准确,适用于脉络宁注射液中25种矿物质元素的同时测定。     

Die Lateralität und Lateralitätsinstabilität in der Diagnostik und Therapie

The disturbance and instability of laterality are obstacles to diagnostics and therapy. Correction prior to starting therapy is required. They also predispose toward defined health problems and unspecific diseases. Numerous research activities provide evidence of the relevance of undisturbed laterality in diagnostics and therapy. Techniques of testing and therapeutic corrections will allow for optimized therapy success.     

Yerba Mate or Paraguay Tea

正Beverages based on Ilex paraguariensis A.St.-Hil.are used in the south Brazil and other Latin American countries located at the so-called southern cone.It is known as chimarro or mate in south and southeast Brazil,tererêin     

Journal of Acupuncture and Tuina Science Instructions for Authors

The Journal of Acupuncture and Tuina Science, a journal with an international scope （IS SN 1672-3597, CN 31-1908/R, Bimonthly）, is embodied by ＇Springer Verlag＇ Database, Index Copernicus （IC） and Chinese Scientific and Technical Paper and Citations Data （CSTPCD）. You can search full text on http：//www, springerlink, com/content/1672 -3597.     

Ethnopharmacologic study of chinese rhubarb

This paper deals with an interdisciplinary study covering historic, botanical, phytochemical, pharmacological and clinical aspects of rhubarb and related species, to lay stress on the correlation between plant phylogeny, chemical constituents and purgative activity.

It was found that the official rhubarbs were exclusively restricted in the Sect. Palmata e.g. Rheum palmatum R. palmatum var. tanguticum R. officinale; the following criteria may serve as their standard, viz., the presence of sennoside derivatives and rhein, the occurrence of the reduced form of rhein and aloe-emodin, the leaves with any kind of palmate incision. Comprehensive multivariate analyses showed that there is a very close relationship between the leaf incision, existence of sennosides or rhein and purgative activity.     

基于ICP-MS法的加味左金丸中无机元素分析

目的 通过电感耦合等离子体质谱（inductively coupled plasma mass spectrometry,ICP-MS）法建立加味左金丸中Cd、Pb、As、Hg、Co、V、Ni、Cu、Li、Sb、Ba、Mo、Sn、Cr、Na、Mg、Al、Ca、Ti、Mn、Fe、Zn、Ga、Se、Sr、Tl共计26种无机元素的测定方法。方法 加味左金丸通过微波消解法处理后,根据相对分子质量的大小选择内标物,其中⁷Li、²³Na、²⁴Mg、²⁷Al、⁴⁰Ca、⁴⁸Ti、⁵¹V、⁵²Cr、⁵⁵Mn、⁵⁶Fe、⁵⁸Ni、⁵⁹Co、⁶³Cu、⁶⁶Zn、⁷⁰Ga、⁷⁵As、⁷⁷Se、⁸⁶Sr以⁷²Ge作为内标;⁹⁵Mo、¹¹⁴Cd、¹¹⁸Sn、¹²¹Sb、¹³⁷Ba以¹¹⁵In作为内标;²⁰²Hg、²⁰⁵Tl、²⁰⁸Pb以²⁰⁹Bi作为内标。对标准品溶液、空白溶液与供试品溶液进行分析,采用标准曲线法进行定量分析。通过ICP-MS法进行测定。结果 26种无机元素线性的相关系数r ≥ 0.999 6,检出限为0.001~1.500μg/L,定量限为0.01~5.00 μg/L,精密度与重复性试验的RSD均小于5%,平均回收率在82.64%~106.44%,RSD均小于5%。对3个厂家的12批样品进行了测定,26种元素的含量差异较大,其中Na、Mg、Ca、Fe 4种元素的含量比较高,均大于500 μg/g,Cd、Pb、As、Hg、Co、Li、Sb、Mo、Sn、Cr、Se、Tl的含量比较低,均小于1 μg/g。由结果可知,人体的常量元素,如Na、Mg、Ca的含量比较高,Cd、Pb、As、Hg等有害元素含量比较低。根据《中国药典》2020年版一部的要求,本品中Cd、Pb、As、Hg与Cu均符合规定。结论 该方法快速、准确,可以用于加味左金丸中无机元素的测定。     

Wirksamkeit der Akupunktur bei der Therapie von idiopathischen Schmeckstörungen: Eine randomisierte Placebo-kontrollierte Studie

Background

At present, the state-of-the-art medication in treating idiopathic taste disorder (gustatory dysfunction) is zinc. If zinc medication was unsuccessful, not tolerated or if it is contraindicated the persons affected can hardly be helped.

Objectives

In a randomized placebo-controlled clinical trial an attempt was made to determine the efficacy of acupuncture.

Methods

The treatment group was treated with acupuncture needles, the placebo group with an inactive acupuncture-laser. Endpoints of the study were changes in the taste test, the quality of life and the severity of symptoms of depression (BDI) as well as mood changes (ZMS). Satisfaction with the success of the respective therapy was also evaluated. Data were collected before and after therapy and again for the treatment group 10 weeks after completion of the treatment period.

Findings

Treatment with real acupuncture showed a significant improvement in gustatory function as well as a significant improvement in psychological symptoms. Greater satisfaction with the treatment results was evident in the treatment group. The treatment results of acupuncture remained stable over a period of ten weeks after completion of the treatment.

Conclusion

Acupuncture was effective in the therapy of idiopathic taste disorders and therefore it is an effective alternative when zinc medication is not tolerated or unsuccessful. But it is also suitable as a therapy of first choice. Acupuncture can be considered as an extension of the therapeutic spectrum in the difficult treatment of taste disorders.     

Erstaunliches Ergebnis einer Schädelakupunktur nach Yamamoto bei Hemihypsarrhythmie rechts

A girl, three and a half years old at the respective date, premature in 25th week of gestation, had been presented. On day three after birth, she had had a IVH III° right and left with severe involvement of parenchyma and other multiple complications, e. a. infant respiratory distress syndrome up to the 42nd day postpartum, and epileptic attacks with apnoeic events.     

Veränderungen der Herzratenvariabilität (HRV) während Low Level Lasernadelakupunktur: Placebokontrollierte Studie an 19 herzgesunden Probanden

Background

Experimental and clinical studies postulate a neurobiological mechanism of acupuncture by modulating central pain systems, neurohormones and -transmitters. It seems to be quite likely that the autonomic nervous system (ANS) plays an important mediating role in this neuromodulation.

Aim

In measuring heart rate variability (HRV), as a non-invasive approach to the ANS-function, the object of this study was to monitor probable acupuncture-induced changes of autonomic balance. The innovative technology of laser-needle acupuncture offers for the first time a stimulation method which fulfils the demands on a placebo-controlled acupuncture trial not requiring controversial sham acupuncture.

Method

19 healthy voluntary subjects underwent 3 treatments in randomized sequence, consisting of placebo-, 1-point- (PC 6) and simultaneous 3-point- (PC 6, LR 3, SI 3) laser-needle-stimulation over 20 minutes. Before, during and after placebo-/verum laser-needle acupuncture, HRV-data for normalized HF(high frequency)- and LF(low frequency)-Power (nHF, nLF) and their quotient nLF/nHF obtained by power spectrum analysis (FFT), were measured and analyzed statistically at 5 different time points (ANOVA repeated measures, p < 0,05).

Results

During both verum applications, the 1-point- (PC 6) as well as the simultaneous 3-point- (PC 6, LR 3, SI 3) laser-needle stimulation, significant changes of the ANS-activity were found in comparison to the placebo application. The most significant modification of HRV was an increase of nHF (p < 0,05 (PC 6), p < 0,0001 (PC 6, LR 3, SI 3)) as an expression of growing vagal activity during acupuncture.

Conclusion

Laser-needle acupuncture causes in 1-point-stimulation (PC 6) as well as in simultaneous 3-point-stimulation (PC 6, LR 3, SI 3) significant changes in HRV in comparison to placebo application. HRV-monitoring seems to be a suitable approach in exploration of acupuncture-induced changes of ANS and could possibly be established in combination with laser needle acupuncture as a standard for further scientific and clinical acupuncture investigations which are greatly needed.