Objective To establish a quantification method of HPLC for determining illegally added auramine O,lemon yellow,carmine,sunset yellow,brilliant yellow,acid red,methyl orange,orange Ⅱ,etythrosine and alkaline orange in Gejie Dingchuan Pills,and validate with LC-MS/MS method.Methods The sample was extracted by 50％ ethanol,and determined by HPLC with a gradient elution of acetonitrile-0.01 mol/L ammonium acetate (contain 0.5％ glacial acetic acid) and the detection wavelength was set at 420 nm and 500 nm.The identification was performed by LC-MS/MS,using a gradient elution of acetonitrile-0.01 mol/L ammonium acetate.The analytes were detected by an electro spray ionization tandem mass spectrometry with dynamic MRM.Qualitation of the auramine O based on the retention time and mass charge ratio.Results The calibration curve of ten dyes showed good linearity and correlation coefficients were all above 0.999,the limits of quantitation for ten dyes in samples were between 0.3-2.8 μg/g,and the average recoveries ranged from 96.3％ to 101.1％ with RSD of 0.6％-1.5％.Auramine O could be detected in 33 of 123 samples.Conclusion LC-MS/MS method is accurate and reliable for the qualitative identification and the HPLC method is simple,rapid and accurate for the content determination.The combination of HPLC and LC-MS/MS can detect ten dyes in Gejie Dingchuan Pills rapidly,accurately and sensitively.

目的:建立天黄猴枣散中胆红素HPIC含量测定方法.方法:采用CAPCELLPAK C18色谱柱(250mm×4.6mm,5μm),以乙腈-甲醇-0.1％磷酸溶液(用三乙胺调节pH值至6.0)(13∶50∶37)为流动相,检测波长451nm.结果:胆红素在0.01931 ～1.9309μg范围内呈良好的线性关系;回收率为100.3％,RSD =2.5％ (n=9).结论:本法专属性强,简便快速,精密度良好.

Objective To establish a HPLC method for the determination of Cassia corymbosa glycoside content in Jingxuening Capules. Methods The analytical column was a Capcellpak-C18 ( 250 mm × 4. 6 mm, 5 μm ) . The mobile phase consisted of methanol-phosphate mixed solution ( dissolving disodium hydrogen phosphate 1. 8 g, potassium dihydrogen phosphate 2. 8 g and heptane sulfonic acid sodium 1. 0 g in water and adding water to 1L, adjusting to pH 6. 0 by phosphoric acid ) ( 25:75 ) . The detection wavelength was 335 nm. The column temperature was 30℃ and the flow rate was 1. 0 mL/min. Results The linear range of Cassia corymbosa glycoside was in the range of 0. 001 991-0. 995 5 μg, r=0. 999 6, the average recovery rate was 99. 08% with RSD 1. 88% ( n=9 ) . Conclusion This method has strong specificity and good repeatability, and is suitable for the content determination of Cassia corymbosa glycoside in Jingxuening Capules.

Objective To investigate the species and distribution of Mussaenda L. in Guangxi, and provide basis for protecting, developing and utilizing the local plant resources. Methods By field survey, specimens collection and identification and literatures consultion, Mussaenda L. in Guangxi was investigated. Results Mussaenda L. in Guangxi contains 8 species, and the majority of them are Mussaenda pubescens Ait.f and Mussaenda eros Champ. Conclusion The investigation results provide some basis for protection, development and utilization of the resources of Mussaenda L. in Guangxi.

Objective:To research pharmacognosy of eight species of Mussaenda L..Method:The chatacters,microscopic identification and TLC were adopted.Result:There were some differences in the morphology from the original plant Mussaenda L.,and there was no obvious difference in characters,microscopic identification and TLC.Conclusion:From the results of the identification of pharmacognosy,the eight species of Mussaenda L.can be used as Mussaenda pubescens for medicine.

Objective:To establish a method for the determination of cholic acid and deoxycholic acid in Tianhuang Houzao powders by HPLC.Method:A C_(18) column was used.The mobile phase consisted of acetonitril -0.2%phosphoric acid solution(48:52) at a flow rate of 1.0 ml·min~(-1).The detection wavelength was 192 nm.Result:There was a good linear range ol 2.04-51.08μg for cholic acid and that of 1.49-74.73μg for deoxycholic acid.The average recovery for cholic acid was 97.8%with RSD of 1.5%(n = 9), and that for deoxycholic acid was 98.7%with RSD of 1.9%(n =9).Conclusion:The method is simple and rapid.It can be used in the determination of cholic acid and deoxycholic acid in Tianhuang Houzao powders.

Objective: To establish method for the determination of 119 pesticides in Astragali Radix by LC-MS/MS.Methods: The sample was extracted by acetonitrile,cleaned by PSA,C18 and graphitized carbon and separated by HPLC.Chromatographic separation was performed on ZORBAX Eclipse plus C18 column(2.1 mm×100 mm,1.8 μm)using a gradient elution of acetonitrile(contain 5% water,0.1% formic acid,5 mmol·L-1 ammonium formate)-water(contain 0.1% formic acid,5 mmol·L-1 ammonium formate)at a flow rate of 0.4 mL·min-1.The column temperature was 40 ℃ and the sample size was 5 μL.The analytes were detected by an electrospray ionization tandem mass spectrometry with dynamic MRM.Qualitation of the pesticides based on the retention time and mass charge ratio and the quantitation based on the peak area of fragment ion.Results: The calibration curve of 119 pesticides was good linear in the range of 0.012-0.75 ng(r 0.9930),and the average recovery of largely analytes were in the range of 70%-120%.The LODs of this method were between 0.003–22 μg·kg-1.Conclusion:This method is accurate and repeatable.It can be applied to screening and detection of these pesticides in Astragali Radix.

OBJECTIVE:To establish the method for the content determination of phillyrin in Bingduqing oral solution.METHODS:HPLC method was used.The Hydro-RP 80A C18(250 mm×4.6 mm,5 μm) column was used with mobile phase consisted of acetonitrile-water(22:78) at the flow rate of 1.0 mL·min-1.The column temperature was 35 ℃ and UV detection was set at 277 nm.RESULTS:The linear range of phillyrin was 0.100 5～2.412 8 μg(r=0.999 9) with an average recovery of 97.21%(RSD=2.1%,n=9).CONCLUSION:The method is simple,accurate and repeatable.It can be used for the content determination of phillyrin in Bingduqing oral solution.

AIM:To establish a solid-phase extraction with high-performance liquid chromatography(SPEHPLC) method for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Weichangning Tablet(Microctis Folium,Polygoni salicifolii Herba,Guajavae Folium,Polygoni Chinensis Herba,Mahoniae Caulis).METHODS: WCX weak cation exchange column was used to SPE.The Hvydro-RP 80A C18 column(250 mm × 4.6 mm,5 μm) was used at 35 ℃ with acetonitrile-0.05 mol/L sodium dihydrogen phosphoric acid(pH2.8)(27 ∶ 73) as the mobile phase,1.0 mL/min as the flow rate,265 nm as the detective wavelength.RESULTS: The linear ranges were 3.443 7-6.887 4 ng(r = 1.000 0) for jatrorrhizine hydrochloride,2.306-23.060 ng(r = 1.000 0) for palmatine hydrochloride and 2.361 3-23.613 5 ng(r = 0.999 7) for berberine hydrochloride.The average recoveries were 99.71%(RSD was 0.85%),100.32%(RSD was 0.98%) and 100.32%(RSD was 1.09%),respectively.CONCLUSION: This method is simple,accurate and reproducible.It can be used for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Weichangning Tablet.

Objective:To establish an HPLC method for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Jinji tablets.Methods:WCX weak cation SPE column was used to clean.The Hvydro-RP 80A C18 column(250 mm×4.6 mm,5 μm)was used at 35 ℃ with acetonitrile-0.05 mol·L-1 sodium dihydrogen phosphate(pH 2.8)(27∶73)as the mobile phase,1.0 mL·min-1 as the flow rate,265 nm as the detective wavelength.Results:The linear ranges were 4.94-49.44 ng(r=1.000)for jatrorrhizine hydrochloride,4.36-43.60 ng(r=0.9999)for palmatine hydrochloride and 3.99-39.94 ng(r=0.9999)for berberine hydrochloride.The average recoveries(n=9)were 98.32%,99.53% and 98.35%,respectively.Conclusion:This method is simple,accurate and repeatable.It can be used for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Jinji tablets.

Objective:To establish an HPLC method for the determination the content and uniformity of ephedrine hydrochloride in gutong plasters.Method:The Kromasil C_(18) column(250 mm×4.6 mm,5μm) was used at 30℃with acetonitrile-0.1%phosphoric acid(5:95) as the mobile phase,1.0 ml·min~(-1) as the flow rate,207 nm as the detective wavelength.Result:The linear range of ephedrine hydrochloride was 0.052 7-2.6350μg,r=1.000 0,the average recovery was 103.07%and RSD was 1.70%(n=6).Conclusion: This method is simple,accurate and repeatable.It can be used for the determination the content and uniformity of ephedrine hydrochloride in gutong plasters.

Objective:To establish an HPLC-ELSD method for determination of sodium taurocholate in shedan chuanbei solution. Method:The analytical column Inertsil ODS-3 C_(18)(250 mm×4.6mm,5μm) was adopted;The mobile phase consisted of acetonitrile (A)-0.003%Triethylamine(B) with the gradient elution,at the flow rate of 1.0 ml·min~(-1);The column temperature was 35℃.The temperature of drift tube was 110℃and the air flow rate was 3.5 L·min~(-1).Result:The linear range of sodium taurocholate was 0.102-1.02μg(r = 0.999 4),the average recovery was 103.69%and the RSD was 1.04%(n=9).Conclusion:this method is simple,accurate and repeatable.It can be used for the determination of sodium taurocholate in shedan chuanbei solution.

Objective To establish an HPLC method for the determination of notoginsenoside R1,ginsenoside Rg1 and ginsenoside Rb1 in Sanqixueshangning powder.Methods The analytical column was an ODS Hypersil C18(4.6 mm ×250 mm,5 μm).The mobile phase consisted of acetonitrile(A)-water(B) with the gradient elution(0-25 min,20%A,25-75 min,20%-35%A).The flow rate was 1.0 mL·min-1 and the column temperature was 35 ℃.The detection wavelength was 203 nm.Results The linear range of notoginsenoside R1 was 0.225-5.625 μg with r=1.000 0,and the average sample recovery was 100.06%.The linear range of ginsenoside Rg1 was at 2.076-20.76 μg with r=0.999 7,and the average sample recovery was 99.92%.The linear range of ginsenoside Rb1 was at 2.056-20.56 μg with r=0.999 8,and the average sample recovery was 96.91%.Conclusion This method is accurate,sensitive and reproducible.It can be used for the quality control of Sanqixueshangning powder.

Objective:To establish an HPLC - ELSD method for determination of notoginsenoside R_1,ginsenoside Rg_1 and ginsenoside Rb_1 in Sanqi Xueshangning capsules.Methods:The analytical column HYPERSIL C_(18)(4.6 mm×250 mm,5μm) was adopted;The mobile phase consisted of acetonitrile(A) -water(B) with the gradient elution [0-25 min,A -B(20:80);25 -75 min,A - B(20:80)→A - B(35:65)],at the flow rate of 1.0 mL·min~(-1);The column temperature was 35℃.The temperature of drift tube was 106℃and the air flow rate was 2.9 L·min~(-1).Results:The linear range of notoginsenoside R_1 was in the range of 0.225 - 5.62μg(r = 1.000),and the average recovery(n =9) was 101.3%;The linear range of ginsenoside Rg_1 was in the range of 2.08 -20.8μg (r =0.9997),and the average recovery(n =9) was 99.9%;The linear range of ginsenoside Rb_1 was in the range of 2.06 -20.6μg(r =0.9998),and the average sample recovery(n =9) was 96.9%.Conclusion:This method is simple and accurate.It has high sensitivity and good repeatability.It can be used for quality control of Sanqi Xueshangning capsules.

目的:对蛞蝓科动物黄蛞蝓进行生药鉴定。方法:采用性状鉴别、显微鉴别和薄层层析鉴别。结果:蛞蝓的组织构造有一定的特征,薄层色谱中斑点清晰,易于识别。结论:可做为该药材质量标准的参考依据。

Objective To establish a HPLC method for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in Chinese Mahonia Stem.Methods The analytical column was the GrcaeSmart C18 Column(250 mm × 4.6 mm,5 μm).The mo-bile phase consisted of 0.05 mol/L potassium dihydrogen phosphate(adjusting pH 3.0 by phosphoric acid)-acetonitrile(70 ∶ 30).The de-tection wavelength was 265 nm.The column temperature was 35 ℃ and the flow rate was 1.0 mL/min.Results The linearity of jatrorrhizine hydrochloride was in the range of 0.03-1.97 μg,r = 0.999 6,the average sample recovery rate was 98.45%;the linearity of palmatine hydrochloride was in the range of 0.04-2.19 μg,r = 0.999 8,the average sample recovery rate was 100.94%;the linearity of berberine hydrochloride was in the range of 0.03-2.12 μg,r = 0.999 9,the average sample recovery rate was 100.29%.Conclusion This method has good repeatability,flexibility and high sensitivity.It can be used for the determination of jatrorrhizine hydrochloride,palmatine hydrochlo-ride and berberine hydrochloride in Chinese Mahonia Stem.

Objective:To establish a solid-phase extraction with high-performance liquid chromatography(SPE-HPLC) method for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in jinji capsules.Method:WCX weak cation SPE column was used to clean.The Hvydro-RP 80A C_(18) column(250 mm×4.6 mm,5μm) was used at 35℃with acetonitrile -0.05 mol·L~(-1) sodium dihydrogen phosphoric acid(pH2.8)(27:73) as the mobile phase,1.0 ml·min~(-1) as the flow rate,265 nm as the detective wave length.Result:The linear range were 4.94-49.44 ng(r = 1.000 0) for jatrorrhizine hydrochloride,4.36-43.60 ng(r = 0.999 9) for palmatine hydrochloride and 3.99-39.94 ng(r = 0.999 9) for berberine hydrochloride.The average recovery were 99.32%(RSD=2.2%),101.78%(RSD = 1.7%) and 103.19%(RSD = 1.5%),respectively(n = 9).Conclusion:This method is simple,accurate and repeatable.It can be used for the determination of jatrorrhizine hydrochloride,palmatine hydrochloride and berberine hydrochloride in jinji capsules.

ObjectiveTo develop an HPLC method for the determination of hesperidin in Baimei Zhike granule.Methods Diamonsil C18 column (5 μm,4.6 mm×250 mm) was used,at 35℃ with methanol-acetic acid-water (35∶4∶61) as the mobile phase,1.0 ml/min as the flow rate,284 nm as the detection wave length.Results The linear range of hesperidin was 0.202～2.020 μg (r=0.9998,n=5),the average recovery was 102.67%,and RSD was 1.42%.Conclusion This method is simple,feasible,and reproducible.It can be used for the quality control of Baimei Zhike granule.

鹿茸、鹿角均为鹿科动物马鹿Cervus elaphus Linnaeus或梅花鹿Cervus nippon Temminck的雄鹿角产品,鹿茸为未骨化密生茸毛的幼角(前者习称为马鹿茸,后者习称为花鹿茸),鹿茸根据外部形态特征可分为二杠和三岔,具有壮肾阳、益精血、强筋骨、调冲任、托疮毒的功效;鹿角为已骨化的角或锯茸后翌年春季脱落的角基(分别称为马鹿角、梅花鹿角、鹿角脱盘),具有温肾阳、强筋骨、行血消肿的功效.本文综述了近年来国内有关鹿茸、鹿角的研究进展.

止血灵胶囊由扶芳藤、黄芪、蒲公英和地榆等4味中药组成.本品对妇科子宫肌瘤出血、恶露不净、经间出血、放环出血、痔疮出血、鼻衄等有良好的疗效.现行标准为国家药品标准WS3-B-3038-98-2004,其含量测定是用薄层扫描法(TLCS)测定黄芪甲苷的含量,但由于该法存在操作较烦琐、影响因素较多、测量误差大及重现性差等不足,而且黄芪甲苷仅在201 nm处附近有弱的末端吸收,采用HPLC法时,一般的紫外检测器检出效果不理想.