1.Study on Quality Standard for Zishen Tongguan Capsules
Dongshun LIU ; Xiaojuan XIONG ; Zhijun WU ; Shujuan PIAO ; Wenquan LU
Chinese Journal of Information on Traditional Chinese Medicine 2016;23(7):104-107
Objective To establish a quality standard forZishen Tongguan Capsules.Methods Anemarrhneae Rhizoma and Phellodendri Chinensis Cortex were qualitatively identified by TLC method. The contents of neomangferin, phellodendrine hydrochloride, mangiferin and berberine hydrochloride inZishen Tongguan Capsules were quantitatively determined by HPLC method.Results The spots of qualitative identification method were clear without interference. Neomangferin in Anemarrhneae Rhizoma and phellodendrinehy drochloride in Phellodendri Chinensis Cortex were identified. Neomangferin, phellodendrinehy drochloride, mangiferin and berberine hydrochloride showed good linearity in the range of 0.025 25–2.02 μg (r=0.999 7), 0.025 5–2.04 μg (r=0.999 7), 0.026–2.08 μg (r=0.999 7), and 0.025 5–2.04 μg (r=0.999 6) respectively. The average recoveries of neomangferin, phellodendrinehy drochloride, mangiferin and berberine hydrochloride were 99.99%, 101.06%, 103.05%, and 100.55%, respectively. The RSD were 2.69%, 5.62%, 2.49%, and 2.06%, respectively.Conclusion The method is accurate and rapid, with good stability, reliability and reproducibility, which can be used for the quality control and evaluation of the preparation of Zishen Tongguan Capsules.
2.Study on Quality Standards forAnshu Liquid
Dongshun LIU ; Wenquan LU ; Shujuan PIAO ; Xiaojuan XIONG
Chinese Journal of Information on Traditional Chinese Medicine 2016;(1):100-102
Objective To establish quality standards forAnshu Liquid.Methods Phellodendri Chinensis Cortex and Kochiae Fructus were qualitatively identified by TLC method. The contents of berberine hydrochloride and phellodendrine hydrochloride in the preparation were determined by HPLC method. The chromatographic column was ZORBAX SB-C18 (4.6 mm×250 mm, 5μm); the mobile phase was acetonitrile-0.1% phosphoric acid (0.5% diethylamine) gradient elution; the flow rate was 1.0 mL/min; the detection wavelength was 284 nm.Results Berberine hydrochloride and phellodendrine hydrochloride in Phellodendri Chinensis Cortex and saponin Ic in Kochiae Fructus were detected by TLC method. The linear relationship of berberine hydrochloride in the preparation was Y=23.109X?30.548,r2=0.999 8, RSD=2.97%, showing that the linear range of berberine hydrochloride was 0.050 5– 2.525 0 μg. The linear relationship of phellodendrine hydrochloride in the preparation wasY=10.038X?2.446 6, r2=0.999 9, RSD=1.24%, showing that the linear range of phellodendrine hydrochloride was 0.050 0–2.500 0 μg. Conclusion The method is accurate, rapid, stable and reliable, with good reproducibility, which can be used for the quality control and evaluation ofAnshu Liquid.
3.Study on Quality Standards for Compound Shatagan Oral Liquid
Shuangying YU ; Xiuhua LIU ; Feng ZHANG ; Shujuan PIAO ; Wenquan LU
Chinese Journal of Information on Traditional Chinese Medicine 2015;22(11):86-88
Objective To establish the quality standards for compound Shatagan Oral Liquid. Methods Chuanxiong Rhizoma was identified by TLC. The content of ferulic acid was determined by HPLC. Separation was performed on a Diamonsil C18 column (4.6 mm × 250 mm, 5μm) with a mobile phase consisting of methanol-1% acetic acid solution in gradient elution (0-5 min, 35% methanol;5-8 min, 35%→23% methanol;8-22 min, 23% methanol) at 30℃;The flow rate was 1.0 mL/min;The injection volume was 5μL;The detection wavelength was 322 nm.Results Ferulic acid showed a good linear relationship in the range of 0.039 4-0.630 0μg (r=0.999 7,n=7). The average recovery was 98.22% and RSD was 2.62% (n=6).Conclusion The method is reliable, sensitive and with repeatability, which can be used as the quality control method for compound Shatagan Oral Liquid.
4.Study on the Quality Standard of Xianrengu Oral Liquid
Jiamei LE ; Xiaojuan XIONG ; Wenquan LU ; Shujuan PIAO ; Feng ZHANG
China Pharmacy 2015;(27):3855-3858,3859
OBJECTIVE:To establish the quality standard for Xianrengu oral liquid. METHODS:Thin layer chromatography (TLC) was used for qualitative identification of Epimedii Folium,Astragali Radix,lycium barbarum,Atractylodes macrocephala and Panax ginseng in Xianrengu oral liquid;RP-HPLC was preformed on the column of Dikma Diamonsil C18 with the mobile phase of acetonitrile-0.1% phosphoric acid (30∶70,V/V)at the flow rate of 1.0 ml/min,the detection wavelength was 270 nm,the temperature was 30℃and the volume was 10μl. RESULTS:TLC identification had good separation,clear spots and high specifica-tion. The linear range of icariin was 7.97-510.00 μg/ml(r=0.999 3);RSDs of precision,stability and reproducibility tests were no more than 0.83%;and the average recovery was 97.69%(RSD=1.30%,n=6). CONCLUSIONS:This method is simple,accu-rate and simple,which can be used for the quality control of Xianrengu oral liquid.
5.Studies on chemical constituents of marine sponge Aplysinopsis sp.
Xue LI ; Shaojiang SONG ; Shujuan PIAO ; Tao DONG ; Houwen LIN
Chinese Journal of Marine Drugs 1994;0(04):-
Five compounds were isolated from marine sponge Aplysinopsis sp.collected from the South China Sea.Their structures were elucidated by ~1H-NMR,~(13)C-NMR and MS as (E)-3'-deimino-3'-oxoaplysinopsin(Ⅰ),(Z)-3'-deimino-3'-oxoaplysinopsin(Ⅱ),3-(2- oxopropyl )- 3-hydroxyind-olin-2-one(Ⅲ),1H-indole-3-carboxaldehyde(Ⅳ),5?,6?-epoxystigmasta -7-en-3?-ol(Ⅴ).CompoundsⅢ,Ⅴwere isolated from Aplysinopsis sp.for the first time.
6.Simultaneous Determination of the Content of 4 Psoralen Compounds in Buwu Tincture by HPLC
Tianyi XIA ; Shun CHEN ; Shouhong GAO ; Chunhua YOU ; Feng ZHANG ; Wenquan LU ; Shujuan PIAO ; Wansheng CHEN
China Pharmacy 2015;26(33):4734-4736
OBJECTIVE:To establish a method for simultaneous determination of 4 psoralen compounds in Buwu tincture. METHODS:HPLC was performed on the column of Dikma Diamonsil C18 with mobile phase of acetonitrile-0.2% Acetic acid by gradient elution at flow rate of 1 ml/min,detection wavelength was 246 nm,column temperature was 30 ℃,and the injection vol-ume was 15 μl. RESULTS:The linear range was 13.00-208 μg/ml for angelicin,26.00-416 μg/ml for bavachin,24.50-392 μg/ml for psoralidin and 37.88-606 μg/ml for isobavachalcone,respectively(r≥0.999 6);RSDs of precision,stability and reproducibility tests were less than 2.00%;recoveries were 95.22%-97.23%(RSD=0.87%,n=6),100.24%-104.64%(RSD=1.62%,n=6), 102.28%-104.39%(RSD=1.47%,n=6)and 97.68%-100.17%(RSD=0.97%,n=6),respectively. CONCLUSIONS:The method is simple and reproducible,and can be used for the quality control of Buwu tincture.
7.Study on quality control of Xinnaoling granules
Xinxin REN ; Xianyou WANG ; Wenquan LU ; Shujuan PIAO ; Shouhong GAO
Journal of Pharmaceutical Practice 2016;34(4):338-342
Objective To establish quality control of Xinnaoling granules .Methods Thin layer chromatography (TLC) methods were used to identify Rhizoma Corydalis ,Radix Angelicae dahuricae ,Cortex Magnoliae officinalis ,Radix Glycyrrhi-zae ,Rhizoma Ligusticum ,Ligusticum wallichii ,Schisandra Chinensis ,Dendranthema morifolium .The concentration of salvi-anolic acid B was determined by high performance liquid chromatography (HPLC) .The method employed a column of Agilent Eclipse XDB-C18 (4 .6 mm × 250 mm ,5 μm) with a mobile phase of 0 .5% formic acid (A)-acetonitrile (B) at a temperature 25℃ .The gradient elution program was as follow :0~5 min 24% B ,5~6 min 24% ~19% B ,6~25 min 19~20% B .The flow rate was 1 .0 ml/min ,and the injection volume was 10μl and the detection wavelength was 286 nm .Results The spots in TLC plates were clear and specific .As for salvianolic acid B ,the linear range was 20-1 280 μg/ml and the equation of linear regres-sion of salvianolic acid B was Y=13 .304 X -117 .50 (r=0 .999 9 ,n=7) .The average recovery rate was 96 .17% (RSD=1 . 10% ) .Conclusion The method was proved to be simple ,reliable ,reproducible ,and could be used in the quality control of Xinnaoling g ranules .
8.Determination of matrine in Lefu oral liquid by HPLC
Xianglei WU ; Ming YUE ; Hao HUANG ; Wenquan LU ; Shujuan PIAO ; Feng ZHANG
Journal of Pharmaceutical Practice 2016;34(5):443-446
Objective To establish a high performance liquid chromatography method for the determination of matrine in Lefu oral liquid .Methods The HPLC method was performed on a Diamonsil Platisil NH2 column (4 .6 mm × 250 mm ,5μm) with the mobile phase of acetonitrile-isopropyl alcohol-3% phosphoric acid solution (84 ∶ 4 ∶ 12 ) . The flow rate was 1 .2 ml/min .The sample injection volume was 5 μl .The detective wavelength was 205 nm .Results The calibration curve of matrine showed good linear response ranged from 54 .50 to 872 .00 μg/ml with r=0 .999 1 .The average recovery of spiked samples for matrine was 99 .82% while the relative standard deviation for repetitions was 1 .12% .Conclusion The method was simple ,reliable and repeatable ,which could be used for the quantitative determination of matrine of Lefu oral liquid .
9.Quality control standard for Qingre Baidu granules
Tianyi XIA ; Bing ZHANG ; Shouhong GAO ; Wenquan LU ; Shujuan PIAO ; Tao PANG
Journal of Pharmaceutical Practice 2016;34(5):450-454
Objective To establish a quality control standard for Qingre Baidu granules .Methods Isatidis Radix ,Fruc-tus Forsythiae ,Herba Violae ,and Glycyrrhizae were identified by TLC ,and the concentration of chlorogenic acid was deter-minedbyHPLC.ThismethodwasemployedonanAgilentZORBAXSB-C18column(4.6mm×250mm,5μm)at30℃ witha mobile phase of acetonitrile (A) and 0 .2% formic acid (B) using the gradient elution program shown as follows :0-12 min , 11%-12% A run at the flow rate of 1 .0 ml/min .The injection volume was 20 μl and the detection wavelength was 327 nm . Results Characteristic spots could be detected by TLC and the specificity of the method was satisfactory .As for chlorogenic acid ,the equation of linear regression of chlorogenic acid was Y=60 .239 4X+9 .096 3 (r=0 .999 9) with the linear range of 6.19-396 .00 μg/ml .The average recovery was 99 .66% (RSD=2 .82% ) .Conclusion The established method is simple ,reli-able ,reproducible ,and can be used for the quantitative determination and quality control of Qingre Baidu granules .
10.A clinical study on transcatheter arterial chemoembolization plus portal vein chemoembolization after partial hepatectomy for patients with hepatocellular carcinoma with portal vein tumor thrombosis
Shujuan SU ; Hong LI ; Shiteng ZHANG ; Hong PIAO
Chinese Journal of Hepatobiliary Surgery 2018;24(4):240-244
Objective To study the short and long term outcomes in patients after partial hepatectomy carried out for primary hepatocellular carcinoma (PHC) with portal vein tumor thrombosis (PVTF) who were treated with transcatheter arterial chemoembolization (TACE) plus portal vein chemoembolization (PVCE).Methods 57 patients who underwent partial hepatectomy for PHC with PVTT were treated with TACE + PVCE.These patients formed the study group.Another 55 such patients who received TACE only were matched by age and gender to form the control group.Blood samples before and after treatment for these 2 groups were collected to study the serum tumor markers.Any chemotherapy-related toxicity and complications were recorded.The hepatocellular carcinoma recurrence rate and recurrence time were recorded on follow up.Survival analysis was conducted.Results There was no significant difference between the two groups in TACE treatment times (P > 0.05).In the study group,the levels of AFP,IGF-Ⅱ,and IGFBP-2 were significantly lower than those in the control group at 1 month after chemotherapy [respectively,(4.3 ± 0.5) μg/L vs.(4.8±0.6) μg/L,(3.3±0.4) μg/L vs.(4.0±0.5) μg/L,(5.3±0.6) μg/L vs.(5.8 ± 0.6) μg/L;all P < 0.05].The range of follow-up of the patients in this study were 9 to 45 months after operation.The 1 year recurrence rate after operation in the study group was significantly lower than those in the control group (28.1% vs.47.3%) (P<0.05).The PFS,OS,2 year and 3 year survival rates were all significantly higher than those in the control group [respectively,(13.4 ± 4.6) m vs.(11.0±3.5) m,(22.6±10.9) m vs.(17.2 ±10.1) m,43.9% vs.25.5%,33.3% vs.16.4%].The differences in the PFS and OS between the two groups were significantly different (P < 0.05).There was no significant difference in the rates in toxicity between the two groups (P > 0.05).In the study group,2 patients (3.5%) developed bleeding from esophageal and gastric fundus vein rupture,while there were no such cases in the control group.Conclusion Compared with TACE alone,the combination of PVCE and TACE after partial hepatectomy for patients with PHC with PVTT effectively reduced tumor burden,prevented liver recurrence and improved long-term survival rates,with no significant increase in toxicity and complication rates.