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Objective:To establish a method which Nifedipine was used as an alternative control for determinating of three flavonoid glycosides in the tablets of Ginkgo biloba leaves by substitution method of reference substance.Methods:Make Nifedipine instead reference substance, the analysis was performed on a JADE-PAK C18 column (4.6 mm × 250 mm, 5 μm), with the mobile phase consisted of 0.5% phosphoric acid solution-methanol (adjusting pH value to 2.2) (50:50) at the flow rate of 1.0 ml/min, the column temperature was 35 ℃. The Nifedipine was selected as the reference substance of three flavonoid glycosides and the correction factor of Nifedipine. The content of total flavonoid glycosides was determined by relative correction factor f and substitute reference.Results:The linear ranges of Nifedipine, quercetin, kaempferide and isorhamnetin were 0.17-1.73 μg, 0.11-1.08 μg, 0.08-0.84 μg, 0.04-0.40 μg. The relative correction factor ( f) between Nifedipine and quercetin, kaempferide, isorhamnetin were 0.782 2, 0.768 5, 0.808 8, respectively. The average recovery ( n=6) were 98.48%, 98.03%, 94.55%. Conclusion:The results indicated that the HPLC method by substitute reference substance is economical, feasible and practical.
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Objective To establish a quantitative method for the simultaneous measurement of the residual level of three pesticides in Nelumbinis semen by GC-MS/MS. Methods The samples were extracted by acetonitrile and purify by Cleanert TPH column. The samples were then tested by GC-MS/MS. Information on relative retention time and mass charge ratio was used for qualitative analysis. The peak area obtained by secondary ion MS of bifenthrin (181.1/166.1)was used as the reference peak to calculate the relative correction factor for the peak area of fenpropathrin (265.1/210.1) and deltamethrin (252.9/93.0), to establish a method using bifenthrin as the reference substance to determinate there sidual quantity of three pesticides in Nelumbinis semen by GC-MS/MS. Results When the injection quantity of the sample containing bifenthrin,fenpropathrin and deltamethrin in the range of 0.01-0.1 ng , there was a good linear relationship between the injection quantity and peak are a Limitation of quantification (LOQ) of bifenthrin , fenpropathrin and deltamethrin were 4.321×10-4 ng, 3.435×10-4 ng, 8.913×10-3 ng, respectively. The average recovery rates of bifenthrin, fenpropathrin and deltamethrin were 93.5％, 93.5％ and 93.8％, respectively. Conclusions The method of quantitative analysis of multi-components with a single-marker is simple, quick and accurate. It suitable for the detection of residual quantity of bifenthrin, fenpropathrin and deltamethrin in Nelumbinis semen.
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Objective To establish a HPLC-MS/MS method for comprehensive monitor and control of the raw material feeding (Gentiana scabra,Katsumade Galangal Seed and dried tangerine peel),and determination of Gentiopicroside,Alpinetin,Cardamonin and Hesperidin in Compound gentian tincture.Methods The separation was performed on an Inertsil ODS-3 (4.6 mm× 150 mm,5 μm) analytical column with the mobile phase consisting of acetonitrile-0.1％ formic acid solution by gradient elution program,and the column temperature was 40 ℃.Active ingredients were separated by HPLC.The Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode,and reactions ion monitoring mode (MRM) for quantitative analysis were selected.Results Through the analysis of the samples with mixed extract the same characteristic peak in MS was found to determine the proprietary Chinese medicine according to the prescription feeding process.The calibration curve of Gentiopicroside,Alpinetin,Cardamonin and Hesperidin were linear:103.26-619.56 μg (r=0.999 0),109.50-657.00 μg (r=0.999 5),105.50-633.00 μg (r=0.996 9),105.02-630.12 μg (r=0.999 5).The precision was Gentiopicroside 0.81％,Alpinetin 0.48％,Cardamonin 0.61％ and Hesperidin 1.55％ respectively.The average recovery rate were Gentiopicroside 95.08％,Alpinetin 93.28％,Cardamonin 94.78％ and Hesperidin 95.04％ respectively.Conclusions The method was proved to be simple,accurate,reliable,high sensitivity and can be used for determination and control of the raw material feeding (Gentiana scabra,Katsumade Galangal Seed and dried tangerine peel).
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Objective The HPLC-MS/MS is used to comprehensively monitor the feeding conditions of raw materials in Yuanhu analgesic capsules, and the content of the index components can be detected at the same time. Methods The Inertsil ODS-3 (4.6 mm×250 mm, 5 μm) was used with the column temperature 40 ℃, Flow phase: 0.1% formic acid-acetonitrile; the gradient elution program, active ingredients were separated by HPLC, and the Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode, and reactions ion monitoring mode (MRM) for quantitative analysis were selected. Results Through analysis and contrast of the medicinal materials, reference substance of primary mass spectrogram showed the same characteristic peak, and the proprietary Chinese medicine can be judged by prescription feeding process. The tetrahydroxene and imperatorin had a good linear relationship in 5.08×10-5-30.45×10-5μg (r=0.999 4), 5.02×10-5-30.09×10-5μg (r=0.999 2). Precision test were 0.99% and 1.14%, the recovery rate were 97.02%-99.66%, 97.62%-99.94%. Conclusions The method is simple, accurate and reliable, high sensitive and fast. It is suitable to monitor the feeding condition and quality of yuanhu analgesic capsules.
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Objective The monitoring of the feeding situation of active pharmaceutical ingredient in Shendan-Chenpi tablet by HPLC-MS/MS,and the content of sodium taurocholate and hesperidin.Methods Using ZORBAX Eclipse Plus C18(4.6 mm×250 mm, 5 μm)Column temperature 40 ℃, Mobile phase with acetonitrile-10 mmol/sodium acetate solution, using gradient elution program. Active ingredients were separated by HPLC, and the Electrospray Ionization Mass (ESI) source was applied and operated in the negative ion mode, and reactions ion monitoring mode(MRM) for quantitative analysis were selected. Results The proprietary Chinese medicine is judged by the prescription feeding process, through analysis and contrast of the medicinal materials, reference substance of primary mass spectrogram, secondary mass spectrogram of peak. The aurocholic acid sodium and hesperidin had a good linear relationship in 0.242×10-2-1.45×10-2μg(r=0.996 0), 0.688×10-2-10.30×10-2μg(r=0.999 2), and the precision test were 0.78% and 1.56%, and the recovery rate were 102%-103%,96%-109%. Conclusions The method was simple, accurate and reliable, high sensitive and fast. The comprehensive monitoring was applied to the Shedan-Chenpi tablet in feeding analysis and quality.
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Objective To study the effects of compound preparations which contain docosahexenoic acid (DHA),soybean lecithin,and vitamin A on memory ability of children and to compare the difference between two compound preparations that contain DHA from marine algae and from fish oil.Methods Totally 160 11-12-year-old healthy children who were studying in a primary school in Baoshan District of Shanghai were enrolled in this study.All the subjects signed the informed consent form.Subjects were randomly divided into three groups with random numbers:marine algae DHA group(n=53),fish oil DHA group(n=53),and control group(n=54).Subjects in the marine algae DHA group were given compound preparation which contained DHA form marine algae,soybean lecithin,and vitamin A;subjects in fish oil DHA group were given compound preparation which contained DHA form fish oil,soybean lecithin,and vitamin A.The dose of DHA(200 mg DHA per capsule)and other components in the two groups was equal.Subjects in the control group were given a placebo with same appearance.The trial lasted 30 days.Each subject took a capsule per day.Immediately before and after the trial,subjects were tested by using the clinical memory scale compiled by the Institute of Clinical Psychology of the Chinese Academy of Sciences.Results Before the trial.there was no difference amongthree groups in terms of all items of clinical memory scale or memory quotient(all P>0.05).After the trial,except for associative learning(both P>0.05),the other items of the clinical memory scale and memory quotient in both marine algae DHA group and fish oil DHA group were significantly higher than those of control group(all P<0.05).No significant difference was noted between the marine algae DHA group and fish oil DHA group for all items of the clinical memory scale or memory quotient(all P>0.05).Conclusions DHA compounds can impreve the memory ability of children.DHAs with different sources have similar effect on memory ability.
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Objective To evaluate the role of lutein in preventing and slowing down age-related macular degeneration (AMD). Methods Literatures concerning lutein and AMD were collected by computerized search, manual search, expert consultations. The quality of included studies was evaluated. RevMan software 4.2was used for meta-analysis. Results Totally 9 studies were included, with a total OR of 0. 81 (range: 0. 71-0.92). Conclusion Lutein can, to some extent, prevent or slow down AMD.
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Objective To investigate the serum levels and dietary intakes of copper, iron, and zinc among adult residents in Dahongshan copper mine area of Yunnan Province in China. Methods Serum levels of copper, iron, and zinc were measured by atomic absorption spectrometry among 180 subjects collected randomly from Dahongshan mine area, among which 171 samples were valid. Dietary intakes of copper, iron, and zinc of 60adults collected randomly from these 180 subjects were detected by chemical analysis. Results Serum levels of copper, iron, and zinc concentrations of 171 valid samples were (0.90±0.18), (1.25±0.93) , and (0.75±0. 28) mg/L, respectively. Serum copper was negatively correlated with serum iron (r = - 0. 26, P ＜ 0. 001). Serum copper was positively correlated with age (r = 0. 25, P ＜ 0. 001). Females had significantly higher serum copper than males (P=0.011). The dietary intakes of copper, iron, and zinc among these 60 subjects were (1.74±1.09),(16.29±10.73), and (7.56±3.38) mg/d, respectively, in which females had significantly lower dietary intakes than nales (all P ＜ 0. 05). Significant regional differences were observed both in serum levels and dietary intakes of copper, iron, and zinc. Conclusions The average serum levels of copper and iron are normal among adult residents in Dahongshan copper mine area, while the average serum zinc level is low. Dietary intakes of these three minerals do not exceed tolerable upper intake levels, and are low in some subjects.