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Objective:To develop the methods for the determination of calcined calamine and borneol in Jinniu ophthalmic remedy. Methods:The content of zinc oxide in calcined calamine was determined by an EDTA coordination titration method. A DB-WAX capillary column (30 m ×0.32 mm,0.5 μm) was used with an FID as the detector and ethylacetate as the solvent to determine the content of borneol. The column temperature was 150 ℃, the injection port temperature was 180 ℃, the detector temperature was 200 ℃, the split ratio was 5 :1,and the flow rate was 1 ml·min-1. Results:The recovery of zinc oxide was 101.5% with the RSD was 1.2%(n = 9). The linear range of borneol was 0.1-5.0 μg(r = 0.999 9). The recovery of borneol was 98.18% with the RSD was 0.8%(n = 9). The content of zinc oxide and borneol in the samples was 0.38-0.59 g·g-1and 0.13-0.21 g·g-1,respectively. Conclusion:The method is simple and accurate with high reproducibility and promising stability, which can be used for the quality control of Jinniu ophthalmic remedy.
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Objective:To determine aflatoxin B1 , B2 , G1 and G2 in Shugan pills by HPLC and evaluate their safety. Methods:The product was analyzed by HPLC using a Shiseido C18 column(150 mm × 4. 6 mm,5 μm)with methanol-acetonitrile-water (10 :30 :60) as the mobile phase. An ultraviolet lamp was derivative at 254 nm, and the fluorescence detection was performed with the excitation wavelength at 360 nm and the emission wavelength at 450nm. The samples from nation-wide market were detected by the method. Re-sults:Good linear relationships were obtained within the range of 10-50 pg for aflatoxin B1 and G1 , and 3-15 pg for aflatoxin B2 and G2 . The recovery of aflatoxin B1 , B2 , G1 and G2 was 89. 9%,87. 9%,86. 1% and 87. 1%,respectively with all the RSD below 3. 0%. The results of all samples were satisfactory, and the qualification rate of the samples was 100%, indicating that the samples were safe. Conclusion:The developed method is convenient and accurate, which can be applied in the quantitative determination of Shugan pills.
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Objective:To determine aflatoxin B1 , B2 , G1 and G2 in Shugan pills by HPLC and evaluate their safety. Methods:The product was analyzed by HPLC using a Shiseido C18 column(150 mm × 4. 6 mm,5 μm)with methanol-acetonitrile-water (10 :30 :60) as the mobile phase. An ultraviolet lamp was derivative at 254 nm, and the fluorescence detection was performed with the excitation wavelength at 360 nm and the emission wavelength at 450nm. The samples from nation-wide market were detected by the method. Re-sults:Good linear relationships were obtained within the range of 10-50 pg for aflatoxin B1 and G1 , and 3-15 pg for aflatoxin B2 and G2 . The recovery of aflatoxin B1 , B2 , G1 and G2 was 89. 9%,87. 9%,86. 1% and 87. 1%,respectively with all the RSD below 3. 0%. The results of all samples were satisfactory, and the qualification rate of the samples was 100%, indicating that the samples were safe. Conclusion:The developed method is convenient and accurate, which can be applied in the quantitative determination of Shugan pills.
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OBJECTIVE:To establish the method for simultaneous determination of epiberberine,jateorhizine hydrochloride, coptisine,palmatine hydrochloride and berberine hydrochloride in Lianshen tonglin tablets. METHODS:HPLC method was adopt-ed. The determination was performed on Thermo Scientific Syncronis C18 column with mobile phase consisted of acetonitrile-0.1%phosphoric acid solution(pH adjusted to 3.0 with triethylamine)(30:70,V/V)at the flow rate of 0.3 mL/min. The detection wave-length was set at 345 nm,and column temperature was 25 ℃. The sample size was 2 μL. RESULTS:The linear ranges were 4.08-163 ng for epiberberine(r=0.9999),5.72-229 ng for jateorhizine hydrochloride(r=0.9998),5.67-227 ng for coptisine(r=0.9999),6.78-271 ng for palmatine hydrochloride(r=0.9996),13.2-526 ng for berberine hydrochloride(r=0.9999). RSDs of pre-cision,stability and reproducibility tests were lower than 2.0%. The recoveries were 96.83%-103.92%(RSD=2.2%,n=9), 97.62%-104.85%(RSD=2.9%,n=9),99.44%-104.18%(RSD=1.8%,n=9), 98.64%-104.42%(RSD=1.8%,n=9), 98.24%-102.40%(RSD=1.5%,n=9),respectively. CONCLUSIONS:The developed method is simple,sensitive,rapid and accu-rate. It is suitable for simultaneous determination of 5 coptis alkaloids in Lianshen tonglin tablets.
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Objective:To establish the specific chromatogram of Fufang Shexiang injection and simultaneously determine five com-ponents( menthol,borneol,patchouli alcohol,muscone,α-asarone) in the injection by GC. Methods:The sample solution was extracted by a solid-phase extraction method. The separation was performed on a DB-WAX GC capillary column with an FID detection. Results:The specific chromatogram had six common peaks, and the similarity was above 0. 91. The five chemical components(menthol,borne-ol,patchouli alcohol,muscone,α-asarone) were well separated and with good linear relationship, the recoveries were between 95. 1 and 102. 6%, and RSD was less than 3. 0%. Conclusion:The method is simple, accurate and reproducible. The specific chromatogram combined with multi-component determination can reflect the overall quality of Fufang Shexiang injection, which can be used for the quality control of the preparation.
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Objective To investigate the clinical efficacy of uterine artery chemoembolization combined with radiotherapy in the treatment of intermediate and advanced cervical cancer.Methods Eighty patients with intermediate and advanced cervical cancer were randomly divided into treatment group and control group by random digits table with 40 patients each.The patients in treatment group were received uterine artery chemoembolization and radiotherapy.The patients in control group were received radiotherapy and intravenous chemotherapy.The short-term efficacy,survival and untoward reaction were observed in 2 groups.Results The complete remission rate and objective response rate in treatment group were significantly higher than those in control group [72.5％(29/40) vs.50.0％(20/40),95.0％(38/40) vs.80.0％(32/40),P ＜ 0.05].There was no significant difference in survival rate of 1,2 and 3-year between the 2 groups (P ＞ 0.05).The incidence rates of leukopenia,anemia,thrombocytopenia,nausea and vomiting in treatment group were significantly lower than those in control group [32.5％ (13/40) vs.67.5％ (27/40),30.0％ (12/40) vs.75.0％ (30/40),7.5％ (3/40) vs.17.5％ (7/40),37.5％ (15/40) vs.70.0％ (28/40),P ＜0.05].There were no significant difference in the incidence rates of radiation cystitis and radiation proctitis between the 2 groups (P ＞ 0.05).Conclusion Uterine artery chemoembolization combined with radiotherapy for intermediate and advanced cervical cancer can improve short-term efficacy and with less side effects.
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Objective To explore the effect of three-dimensional conformal radiation dose fractionation treatment of advanced non-small cell lung cancer(NSCLC).Methods 75 NSCLC patients were treated with hypofractionated 3DCRT( observation group),while 73 cases were treated with conventional fractionated radiotherapy (control group).The efficacy and adverse reactions were observed;Survival after treatment were followed up in 1,2,3 years.Lung function was detected before and after radiotherapy treatment,including FVC,FEV1 and CLCO.Results The total effective cases of control group were 47 cases patients ( 64.4％ ),observation group's was 60 cases ( 80.0％ ),total effective rate had statistically significant difference ( x2 =4.50,P ＜ 0.05 ).Survival of control group after treatment in 1,2,3year were 50.7％,24.7％,8.2％,the median survival was 13 months,observation group's were 73.3％,45.3％,20.0％,and 19 months.The survival of these two groups was statistically different (x2 =8.07,6,94,4.22,all P ＜ 0.05 ).The patients blood system side effects of observation group were significantly lower than the control group ( x2 =4.73,P ＜0.05 ) ;acute radiation pneumonia,esophagitis of these two groups had no significant difference in the incidence( P ＞ 0.05 ).Conclusion Hypofractionated 3DCRT treatment of advanced NSCLC had good effect,and its adverse reactions was low,and it was worthy of clinical application.
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Objective To investigate the clinical effect of hyper-fractionated three-dimensional conformal radiotherapy (3DCRT) combined with transcatheter arterial chemeembolization (TACE) for heating patients with inoperable primary liver cancer.Methods One hundred and two patients with inoperable advanced primary liver cancer were divided by random digits table method into control group with 49 cases treated with TACE and observation group with 53 cases treated with hyper-fractionated 3DCRT combined with TACE.The short-term efficacy,adverse reaction and survival rate of the 1st,2nd and 3rd year and serum alpha-fetoprotein (AFP) expression after treatment in two groups were observed.Results The complete remission rate,progress rate and total efficiency were 17.0％ (9/53),11.3％ (6/53),73.6％ ( 39/53 ) in observation group,2.0％( 1/49 ),28.6％ (14/49),51.0％(25/49 ) in control group.There were significant differences between two groups (P ＜ 0.05).There was no statistical significance in adverse reactions between two groups ( P ＞ 0.05 ).The survival rates of the 1 st,2nd and 3rd year in control group were 51.0％ ( 25/49 ),28.6％(14/49),14.3％(7/49),the median survival time was 15 months;while those in observation groupwere 71.7％(38/53),52.8％(28/53),39.6％(21/53) and 20 months.The survival rates of the 2nd and 3rd year in observation group were significantly higher than those in control group respectively (P ＜0.05 or ＜0.01 ).The rate of patients with no obvious serum AFP protein change between observation group [ 9.8％(4/41) ] and control group [ 31.6％(12/38) ] had statistical significance (P ＜ 0.05).Conclusion Hyper-fractionated 3DCRT combined with TACE for treating patients with inoperable primary liver cancer has good clinical efficacy,it is worthy of clinical practice.
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The paper is to establish a method for simultaneous determination of 5 kinds of alkaloids in ephedra and poppy which are in Kechuanning tablets. Solid-phase extraction (SPE) was adopted in pretreatment, and a UPLC method with 2 different wavelengths had been developed: 210 nm for the detection of morphine, codeine phosphate, ephedrine hydrochloride and pseudoephedrine hydrochloride, and 251 nm for papaverine hydrochloride. The column used was Acquity UPLC BEH C18 (100 mm x 2.1 mm ID, 1.7 microm) with linear gradient elution using acetonitrile and 0.1% phosphoric acid. The flow rate was 0.4 mL.min-1, and the column temperature was 30 degrees C. The linear response range was 0.375 0 - 12.50 microg.mL-1 for morphine, 0.064 32 - 2.144 microg.mL-1 for codeine phosphate, 0.030 06 - 1.002 microg.mL-1 for papaverine hydrochloride, 1.126 - 37.52 microg.mL-1 for ephedrine hydrochloride, 0.287 8 - 9.592 microg.mL-1 for pseudoephedrine hydrochloride (r = 0.999 7). The average recoveries of these compounds were 99.26%, 100.6%, 95.29%, 100.1% and 97.48%, respectively. This is a more reasonable and credible method of quality control for Kechuanning tablets.
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OBJECTIVE: To analyze the uncertainty of determination of western medicine composition illegally added into Chinese patent drug and find out the effect factors of uncertainty in order to provide scientific basis for evaluating test report. METHODS: Antler tablets were tool as example. Qualitative analysis of additive composition was carried out using HPLC-MS method and the content of sildenafil citrate in each tablet was determined. Uncertainty of test was evaluated according to the regulation specified in Evaluation and Expression of Measurement of Uncertainty (JJF1059-1999). RESULTS: The uncertainty of the test is 0.10 mg in each tablet. CONCLUSION: The uncertainty of the experiment is mainly caused by non homogeneity of sample.