ABSTRACT
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.
ABSTRACT
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 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 To develop a HPLC-MS/MS method for comprehensive monitoring and control of the raw material feeding (honeysuchle flowers extract and baikal skullcap root extract) , and simultaneous determination of chlorogenic acid and baicalin in Yinhuang capsules. Methods The separation was performed on an Inertsil ODS-3 (2.1 mm × 150 mm, 5 μm) analytical column with the mobile phase consisting of methanol- 10 mmol/L ammonium acetate solution by gradient elution program, and the column temperature was 40 ℃. Active ingredients were separated by HPLC, and the Electrospray Ionization Mass (API) source was applied and operated in the negative ion mode, and reactions ion monitoring mode (MRM) for quantitative analysis were selected. Results The samples and the mixed Extract have the same characteristic peak in MS and MS/MS. According to the prescription feeding process, the proprietary Chinese medicine wasdetermined. The results showed that the palladium residue of 6 batches samples were up to the standard by HPLC/MS/MS chromatographic peak areas. The calibration cruve of chlorogenic acid and baicalin were linear: 0.60-4.80 μg/ml (r = 0.9989),2.87-14.40 μg/ml (r = 0.9986), with the relative standard deviation of repeatability by 0.69% and 0.69% respectively, and the mean recovery rate were 95%-102%, 95%-103%, respectively. Conclusions The method was proven to be simple, accurate, reliable, high sensitive and can be used for determination and control of the raw material feeding (honeysuchle flowers extract and baikal skullcap root extract) and quality in Yinhuang capsules.
ABSTRACT
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.