Distribution and correlation of 20 kinds of inorganic elements in Jiawei Xiaoyao Formula / 药物评价研究

Objective To study the distribution and correlation of 20 kinds of inorganic elements (Na,Mg,A1,V,Cr,Co,Fe,Ni,Cu,Zn,Mn,As,Se,Cd,Cs,Sr,Ag,Hg,Pb,and U) in Jiawei Xiaoyao Formula (JXF).Methods The levels of 20 inorganic elements in 10 kinds of herbal substances were determined by ICP-MS with microwave digestion for sample preparation,and the results were analyzed with SPSS22.0.Results There were some correlations among the inorganic elements in JXF;Four main factors were selected by principal component analysis (PCA).The PCA results showed that Na,Mg,A1,V,Ni,Cu,Se,Sr,Cs,Mn,Hg,and Fe might be the characteristic elements in JXF;There were Mg,A1,Mn,and Fe elements in 10 herbal drugs,the contents of inorganic elements in herbal drug were different because the medicinal parts were different,and the decreasing order was roots and rhizomes,skin type,all grass,fruit seeds,and fungi.Conclusion Contents of inorganic elements can not only characterize the stability of extraction process,and can provide experimental evidence for the study of traditional Chinese medicine compound compatibility law.

Rapid Determination of Multi-maker Ingredients in Salvia miltiorrhiza by Near Infrared Diffused Reflection Spectroscopy / 中国药房

OBJECTIVE:To establish the method for rapid determination of nuezhenoside in Salvia miltiorrhiza.METHODS:The contents of salvianolic acid B,rosmarinic acid,lithospermic acid and tanshinone (tanshinone Ⅱ A+tanshinone Ⅰ +cryptotanshinone) were determined by HPLC (as reference value).Quantitative model for the contents of above components was established by partial least square (PLS)-NIR spectra.According to the reference value,143 samples were collected and the spectrum was pretreated by first-order derivative.The optimal range of wave band for salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 6 773.98-3 981.12,6 670.85-3 996.54,8 544.66-3 936.28,8 188.06-3 875.31 cm-1.RESULTS:The methodology for the content determination of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were in line with the requirement.The coefficient (R2) of internal cross validation for quantitative correction model of salvianolic acid B,rosmarinic acid,oxalic acid and tanshinone were 0.919 0,0.832 2,0.821 5,0.925 6.The deviation of corrected mean square roots were 4.46,0.48,1.34,0.71,respectively.The R2 values of external validation were 0.852 6,0.957 3,0.819 3,0.953 1,respectively;and mean square root of prediction error (RMSEP)were 9.77,0.28,0.94,0.63,respectively.CONCLUSIONS:The method is rapid,accurate,simple and pollution-free,and can be used for rapid determination of multi-maker ingredients in S.miltiorrhiza.

Study on Contents Determination and Transport Rates of 18 Toxic Elements from 10 Ingredients of Modi-fied Xiaoyao Formula and Their Extracts / 中国药房

OBJECTIVE:To establish a method for simultaneous determination of 18 toxic elements from 10 ingredients of Modified xiaoyao formula and their extracts,and to study transport rates of above elements. METHODS:Microwave digestion-in-ductively coupled plasma mass (ICP-MS) was used to determine above elements. Radio-frequency power was 1.50 kW,atomiza-tion pressure was 720 kPa,sampling depth was 7 mm,plasma gas flow rate was 15.0 L/min,carrier gas flow rate was 1.00 L/min, spray chamber temperature was 2℃,He flow rate was 4.5 mL/min under collision mode,measurement points/peak was 3,data ac-quisition mode was jump mode. RESULTS:The linear ranges of As,Pb,Cu,Hg,Cd,Mo,V,Cr,Mn,Fe,Ni,Zn,Ru,Rh, Pd,Os,Ir,Pt was 0-500.17 ppb(r was 0.9994-09999);LOD was 0.0004-5.3410 ng/g;RSD of repeatability tests was all lower than 5.0%;average recoveries were 82.0%-117.9%(RSD=0.2%-5.7%,n=9). Ru,Rh,Pd,Os,Ir,Pt,Hg had not been detect-ed. The transfer rates of 11 metals in the extracts ranged 1.46%-31.90%. CONCLUSIONS:The method is simple,precise,stable and repeatable,and can be used for simultaneous determination of 18 toxic elements in 10 ingredients of Modified xiaoyao formula and their extracts. The contents of toxic elements are decreased during the preparation of Modified xiaoyao formula extract to guar-antee the safety of drug use to certain extent.

Effect of determination of metals in Cardeniajasminoides Ellis by ICP-MS from online internal standard solution / 药物评价研究

Objective To provide a proper concentration of Internal Standard Solution by comparing five different degrees to the simultaneous analysis of 10 metals including V,Cr,Mn,Fe,Ni,Cu,As,Cd,Pb and Hg in Cardeniajasminoides.Method An Inductively Coupled Plasma-Mass Spectrometry method with Microwave-Assisted Digestion was developed with10,50,200,500,1 000 μg/L of Ge,In,Bi as internal standard.Result The degree of 500 μg/L concentration of internal stand solution can both correct the matrix effect and alleviate the contamination as the 1 000 μg/L.Conclusion With excellent detection limits,high sensitivity and wide linear range,the 500 μg/L internal standard may serve as reference in the determination of elements in other traditional Chinese medicine (TCM).

Research progress in fingerprint of Compound Danshen Dripping Pills and its raw materials / 药物评价研究

Compound Danshen Dripping Pills has curative effect of angina pectoris,coronary heart disease,and other cardiovascular and cerebrovascular diseases,which is widely used in clinic.With the development of basic research and clinical pharmacology,it is particularly important to carry out more comprehensive and systematic quality control.At present,fingerprint technology is developing rapidly and has been recognized by many countries.In this article,we summarized the research situation of Compound Danshen Dropping Pills and its raw materials from two aspects of chromatography and spectroscopy (such as LC,CE,IR,NMR and so on).It will provide reference or the further establishment of a reasonable quality control method.

Compatibility Stability of Salvianolic Acid for Injection Combined with 8 Kinds of Common Solvents / 中国药房

OBJECTIVE:To investigate the compatibility stability of Salvianolic acid for injection (SAFI) combined with 8 kinds of common solvents. METHODS:Referring to package inserts,SAFI was collected and combined with 0.9% Sodium chlo-ride injection,5% Glucose injection,10% Glucose injection,Compound sodium chloride injection,Mannitol injection,Glycerol fructose and sodium chloride injection,Sodium lactate Ringer's injection,Glucose and sodium chloride injection,250 mL each re-spectively,and then sealed in the dark at the room temperature. The appearance of mixtures were observed,pH value,the number of insoluble particles,maximal absorption wavelength and maximal absorbance were detected,and the contents of salvianolic acid B,rosmarinic acid,lithospermic acid and salvianolic acid Y in mixtures were determined by HPLC at 0,1,2,4,8 h after mix-ing. RESULTS:Under above condition,no obvious change was found in appearance or pH values of the mixtures within 8 h. Maxi-mal absorption wavelength ranged 284.5-286.0 nm. After mixed with Mannitol injection,the number of particles≥10μm(1-8 h af-ter mixing)and particles ≥25 μm(4-8 h after mixing)exceeded the scope of Chinese Pharmacopoeia(2015 edition);the maxi-mal absorbance changed significantly(RSD=9.17%,n=5);the relative content of salvianolic acid B,rosmarinic acid,lithosper-mic acid and salvianolic acid Y decreased by more than 10%(RSD=14.65%,6.45%,8.97%,12.49%,n=5);after mixed with Sodium lactate Ringer's injection,the relative content of rosmarinic acid and lithospermic acid changed greatly (RSD=14.57%, 7.28%,n=5);after mixed with 5% Glucose injection(4-8 h after mixing)and Glycerol fructose and sodium chloride injection(8 h after mixing),the relative content of rosmarinic acid were less than 90%(RSD=6.30%,4.86%,n=5);and the number of particles ≥25μm exceeded the scope of phamcopoeia after mixing with Glycerol fructose and sodium injection(0 h). The number of insoluble particles in other mixtures were in line with the standard of pharmacopoeia;maximal absorbance had no significant change(RSD<5%,n=5),and the relative content change of analytes were all less than 10%. CONCLUSIONS:Clinical appli-cation of SAFI combined with Mannitol injection,Sodium lactate Ringe's injection and Glycerol fructose and sodium injecrion should be avoided. After mixed with 5% Glucose injection,SAFI should be used within 4 h. SAFI can be compatible with 0.9%Sodium chloride injection,10% Glucose injection,Compound sodium chloride injection and Glucose and sodium chloride injec-tion.

Research of the Variation Rule and Influencing Factors of 5-hydroxymethylfurfural in the Extraction Pro-cess of Schisandra chinensis / 中国药房

OBJECTIVE:To explore the content variation rule and influencing factors of 5-hydroxymethylfurfural(5-HMF)in the extraction process of the herbs Schisandra chinensis and improve the quality of monitoring the extract of Schisandra chinensis. METHODS:High performance liquid chromatography was adopted to determine the contents of 5-HMF in the extracts during the extraction process (decoction,vacuum concentration,alcohol precipitation,vacuum drying,alkali adjustment),and the content variation rule was found out. For vacuum drying during which the content of 5-HMF reduced obviously,the effects of the tempera-ture and time of drying on the content of 5-HMF were studied,and the effects of vacuum drying and freeze drying on the 5-HMF contents were compared. RESULTS:The content variation trend in the extraction process of Schisandra chinensis was as follows as a large amount of 5-HMF was produced in the herbs decoction process;the content of 5-HMF increased during concentration,re-duced during the alcohol precipitation and the vacuum drying of the extracts by three times concentrate,and maintained substantial-ly unchanged during alkali adjustment. In the process of vacuum drying,the content of 5-HMF decreased with temperature rise and time extension. Freeze drying had no effect as good as that of vacuum drying in the reduction in the content of 5-HMF. CON-CLUSIONS:It is suggested that the vacuum drying of the extracts by three times concentrate at higher temperature,which may pro-duce the extract of Schisandra chinensis with lower content of 5-HMF and thus improve the quality of Schisandra chinensis extract.

Comparison on appearance and non-ginsenoside composition in Panax ginseng and its products processed from different producing areas in northeast China / 中国中药杂志

<p><b>OBJECTIVE</b>To investigate the appearance and moisture, ash content, extract, volatile oil of Panax ginseng and its processed products from different producing areas of northeast China, and thus provide the useful reference data for its quality standard establishment and standardized cultivation.</p><p><b>METHOD</b>Base on the Chinese Pharmacopoeia and literatures relating to P. ginseng, the content of moisture, ash, extract, volatile oil in P. ginseng and its processed products from northeast 10 different producing areas were measured, and data analysis of these various indicators was carried out by DTOPSIS.</p><p><b>RESULT</b>The samples from Changbai, Jian Kangmei and Fusong reached the standard of Chinese pharmacopoeia and national standard, and in addition comprehensive evaluation indicators of them were higher than others samples.</p><p><b>CONCLUSION</b>The quality of ginseng from different producing areas appears very different. Some samples failed to reach the standard of Chinese pharmacopoeia and national standard. Ginseng samples from those 3 producing areas of GAP planting bases showed good quality, which reflects the importance of GAP for ginseng cultivation.</p>

Evaluation methods for quality volatility about yiqi fumai freeze-dried powder used for injection based on bio-thermodynamics exosyndrome / 中国中药杂志

Yiqi Fumai freeze-dried powder for injection was used as a model drug to establish an evaluation method mainly based on bio-thermodynamics profile detection. Fischer function was used to analyze the chemical and biological data In general, chemical chromatogram can distinguish the expired sample and thermal spectrum of biological activity can distinguish special samples exactly. Thus, we established the evaluation method regarding the quality volatility of Yiqi Fumai freeze-dried powder for injection. The method can be used as a useful supplement in quality control as, and it could provide some technical information for quality control of other varieties of traditional Chinese medicine for injection.

Determination of total content of ten ginsenosides in yiqifumai lyophilized injection by near infrared spectroscopy / 中国中药杂志

<p><b>OBJECTIVE</b>To determine the total content of 10 ginsenosides in Yiqifumai lyophilized injection by near infrared spectroscopy.</p><p><b>METHOD</b>Sixty samples were collected and determined of the total contents of ten ginsenosides by HPLC. The optimal calibration model was established by the contents of 10 ginsenosides in fifty samples and their NIR spectroscopy using the PLS. And the contents of 10 samples were successfully predicted.</p><p><b>RESULT</b>When using the pretreatment of the first derivative and MSC in the range of 4 246.8 - 4 602.2, 5 446.8 - 61 02.6 cm(-1), the best dimension was 9, and the quantitative model was accurate. The R2 was 94.2, and the RMSECV was 0.186. The RMSEP of ten samples was 0.234.</p><p><b>CONCLUSION</b>This method is easy, rapaid and precise, and can be used to determine the content of 10 ginsenosides in Yiqifumai lyophilized injection.</p>

Influence of different processing method and mature stage on main chemical constituents of Schisandra chinensis / 中国中药杂志

<p><b>OBJECTIVE</b>To study different processing method and mature stage on the quantity of the Schisandra chinensis in the Xinbin region of Liaoning.</p><p><b>METHOD</b>The schisantherin A and 5-hydroxymethylufrurfal (5-HMF) content in S. chinensis was determined by using the HPLC method. The organic acids content was determined by potentiometric titration. The polysaccharide content was determined by oxidation reduction titration. The volatile oil content was determined by steam distillation.</p><p><b>RESULT</b>The quantity of S. chinensis was different due to different processing method and mature stage.</p><p><b>CONCLUSION</b>The different processing method and mature stage have significant influence on the quantity of S. chinensis.</p>

Study on technology in preparation of Fructus Auranti extract / 中国中药杂志

<p><b>OBJECTIVE</b>To optimize the method of Fructus Auranti extracts preparation.</p><p><b>METHOD</b>The extraction conditions and resin type were examined by using naringin as main indices. The sampling amount, the elution solvent and their flow rates were optimized. The recycling times and recovery capacity of resin were also studied.</p><p><b>RESULT</b>The best extraction could be obtained by adding 10 times amount of NaOH (pH 11) for 3 times, 1 hour each time. The purification conditions were specified as follows: using D101 macroporous resin, the sampling ratio of resin weight to raw material was 1:0.8 with a flow rate of 2 BV x h(-1) and 4 BV 50% aqueous ethanol as elusion solven.</p><p><b>CONCLUSION</b>By using this method, the naringin in the product could reach above 30%. Besides, the optimum method is simple and practical.</p>

Dissection of differences and similarities of botanical drugs in European Union, US and Canada / 中国中药杂志

Because of the unique nature and treatment concept of traditional Chinese medicines (TCMs), TCMs have been respected again since 70s of last century. The regulatory agencies of some developed countries (the FDA, EMA and Health Canada etc) have published new guidance/guidelines/directives in recent years, such as the botanical drug product guidance of the FDA, the evidence for quality of finished natural health products guidance of the Health Canada and the guideline on quality of herbal medicinal products/ traditional herbal medicinal products of the EMA etc. All of the regulatory agencies are willing to scientifically evaluate the herbal medicines and accept it as therapeutic product. This paper analyzed the history of herbal medicine regulation and the similarities and differences of the regulatory requirements of the European Union, the United States and Canada, proposed possible future direction of the international development of Chinese medicine from the perspective of global regulatory affairs.

Simultaneous determination of 4 nortriterpenoids in Schisandra chinensis extract by HPLC / 中国中药杂志

<p><b>OBJECTIVE</b>To determine 4 nortriterpenoids (de-hydroxy arisanlactone D, 25-hydroxy schindilactone, schindilachone A, lancifodilactone D) in Schisandra chinensis extract by HPLC.</p><p><b>METHOD</b>The analysis was performed on a waters symmetry column (4.6 mm x 250 mm, 5 microm) with the mobile phase of acetonitrile-water (33:67) at a flow rate of 1 ml x min(-1). The column temperature was set at 37 degrees C, and the detector wavelength was 264 nm.</p><p><b>RESULT</b>The linear ranges of de-hydroxy arisanlactone D, 25-hydroxy schindilactone, schindilachone A, and lancifodilactone D are 0.075-1.800, 0.098-0.980; 0.095-0.950, and 0.053-0.530 microg, respectively, and the average recoveries were 98.57%, 96.44%, 97.96%, and 97.27%, respectively.</p><p><b>CONCLUSION</b>The four nortriterpenoids were well separated by this method, and it could be used to determine the four nortriterpenoids in Schisandra chinensis extract.</p>

Expression of Tbx3 gene in breast cancer tissues and its clinical significance / 中国医师进修杂志

Objective To clarify the expression of Tbx3 gene in breast cancer tissues and its clinical significance, and the expression of Tbx3 gene in different clinical pathological characteristic breast cancer. Methods Expression of Tbx3 gene in 53 specimens of breast cancer and 28 specimens of normal breast tissues were investigated by immunohistochemistry, analysing the clinical significance. Meanwhile the correlation of expression of Tbx3 gene in breast cancer classified was investigated by estrogen receptor ( ER),lymph node metastasis, Her-2 status. Results Positive rate of Tbx3 gene in breast cancer tissues was significantly higher than that in normal breast tissues [73.58% (39/53) vs 14.29% (4/28)] (P ＜ 0.05).Positive rate of Tbx3 gene in ER positive breast cancer tissues was higher than that in ER negative breast cancer tissues [ 84.38% (27/32) vs 57.14% ( 12/21 ) ] (P ＜ 0.05 ). Positive rate of Tbx3 gene in breast cancer tissues with lymph node metastasis was higher than that in breast cancer tissues without lymph node metastasis [86.21%(25/29) vs 58.33% (14/24) ] (P ＜ 0.05). Positive rate of Tbx3 gene in Her-2 positive breast cancer tissues was higher than that in Her-2 negative breast cancer tissues[ 93.75%(15/16) vs 64.86% (24/37) ] (P ＜ 0.05). Conclusions Tbx3 gene is over expressed in breast cancer tissues. It is related to ER, lymph node metastasis, Her-2 status.

Residuals of organochlorine pesticides and heavy metals in Radix Ophiopogonis and Ophiopogon japonicus growing soil / 中国中药杂志

<p><b>OBJECTIVE</b>To determine the residues of organochlorine pesticides and heavy metals in Radix Ophiopogonis and Ophiopogon japonicus.</p><p><b>METHOD</b>The residues of 4 isomers of benzene hexa chloride (BHC) and 4 isomers of dichloro dipheny trichloroethane (DDT) were determined by gas chromatography. The contents of Pb, Cd, Cu, Cr, Hg and As were determined by ICP.</p><p><b>RESULT</b>The residues of organochlorine pesticides in Radix Ophiopogonis were lower than the permissible maximum limits of the Chinese national standard except hexachloride (BHC) in Radix Ophiopogonis from Cixi as well as Cu in soil of Luojiang.</p><p><b>CONCLUSION</b>The enrichment capacity of Radix Ophiopogonis for (BHC) and Hg is higher. It is suggested that we should try to select herbs-growing soil for O. japonicus with a particular emphasis on the pesticides residues in soil.</p>

Research on chromatographic fingerprint of fruits of Schisandra chinesis / 中国中药杂志

<p><b>OBJECTIVE</b>To study the chromatographic fingerprint of the fruits of Schisandra chinensis, and identify the peaks.</p><p><b>METHOD</b>Analysis was performed at 30 degrees C on a Waters Symmetry C18 column (4.6 mm x 250 mm, 5 microm), eluted with acetonitrile-water gradient elution. The flow-rate was 1.0 mL x min(-1), and detection wavelength was 218 nm. The peaks in the chromatogram were identified by LC-MS.</p><p><b>RESULT</b>The fingerprint of the fruits of S. chinensis was established, and fifteen peaks of lignans were identified.</p><p><b>CONCLUSION</b>The method was easy, reliable and could be used as a powerful tool for the further quality control of S. chinensis.</p>

Quality evaluation of Schisandra chinensis at different producing areas in northeast China / 中国中药杂志

<p><b>OBJECTIVE</b>To investigate the quality of Schisandra chinensis, and thus provide the useful reference data for its quality standard establishment and standardized cultivation.</p><p><b>METHOD</b>Base on the Chinese Pharmacopoeia and literature relating to S. chinensis, the appearance, water-soluble extractive, total ash, acid-insoluble ash and volatile oil of 10 S. chinensis sampes collected from different producing sites in northeast China were studied or determined, and the contents of major active lingans were measured by HPLC.</p><p><b>RESULT</b>The content of total ash and acid-insoluble ash in S. chinensis was less than 7.0%, 1.0%, respectively. The contents of water-soluble extractive were higher than 45.0%. HPLC analyses showed that the content of schisandrol A was higher than 0.40%. All these results in accordance with the requirements of Chinese Pharmacopoeia were published in 2010.</p><p><b>CONCLUSION</b>The differences of the appearance and the internal quality are different for the samples collected from different areas. And the establishment of a scientific and comprehensive quality standard system will be very important role in ensuring the quality of S. chinensis.</p>

Effects of soil factor on active components of Radix Ophiopogonis / 中国中药杂志

<p><b>OBJECTIVE</b>To study the effects of soil factors on the active components in Radix Ophiopogonis.</p><p><b>METHOD</b>The content of polysaccharide, flavonoids, saponins, water-soluble extract and inorganic elements in Radix Ophiopogonis gathered from 7 different places were compared, physical and chemical properties and inorganic elements of soil were analyzed. The path and grey connection analysis were applied for studying the effects on the active components of Radix Ophiopogonis.</p><p><b>RESULT AND CONCLUSION</b>The concentrations of mineral elements in plant were mainly adjusted by active absorption. The active components in Radix Ophiopogonis was primarily effected by soil enzyme activity, the other important factors were potassium, pH, and organic matter. K, Fe, Mn, B, Ba, Zn of soil also had much influence on it then others inorganic elements.</p>

Callus induction of Cinnamonum camphora and formation of borneol / 中国中药杂志

<p><b>OBJECTIVE</b>To optimize the condition of callus of Cinnamonum camphora induced.</p><p><b>METHOD</b>GC and plant tissue culture method were applied in the study.</p><p><b>RESULT</b>The effect of callus induced and the growth of callus were different in MS medium with different proportion of hormone. The ration of callus induced was the highest and the growth of callus was the most prosperous in the MS medium with 4 mg x L(-1) 2,4-D and 0.2 mg x L(-1) 6-BA. It is found that callus induced by young leaf contained borneol, but callus induced by young stem not.</p><p><b>CONCLUSION</b>The optimization of callus of C. camphora induced is using the MS medium with 4 mg x L(-1) 2,4-D + 0.2 mg x L(-1) 6-BA. Callus induced by young leaf can generate borneol.</p>