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Objective To establish an HPLC method for determination of low-molecular-weight carbonyl compounds in the oil-containing herbs. Methods After carbonyl compounds in the samples were extracted with water, the solution reacted with 2, 4-dinitrophenylhydrazine (DNPH) in an acidic medium to form 2, 4-dinitrophenylhydrazone derivatives, which were separated on Kromasil KR100-5 C18 column (250 mm× 4.6 mm, 5 μm). The mobile phase A was water-acetonitrile-tetrahydrofuran-isopropanol (59∶30∶10∶1), mobile phase B was water-acetonitrile (35∶65), gradient elution. The flow rate was 0.8 mL/min, detection wavelength was 365 nm, and column temperature was 30 ℃. Results Good linearities were obtained in corresponding concentration ranges, with correlation coefficient over 0.999. The limits of detection of the eight DNPH derivatives were 0.002-0.008 μg/mL, and the average recoveries were 88.49%-93.65%. Conclusion The method is simple, accurate and reliable, with good reproducibility.
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Objective To establish a capillary gas chromatography method for the determination of menthol and methyl salicylate in Shangtongning adhesive plaster. Methods The internal standard substance of n-Pentadecane was employed. The GC system consisted of a DB-WAX capillary column (30 m?0.32 mm, 0.25 ?m), nitrogen as the carrier gas, column temperature at 130 ℃, FID as the detector at 200 ℃, and with a split ratio of 12∶1. Results The contents of menthol and methyl salicylate in 6 lots of samples were determined and the constituents concerned were separated well under the chromatographic condition. The average recovery of menthol and methyl salicylate were 101.52% (RSD=2.66%) and 100.34% (RSD=3.38%), respectively. Conclusion The method was sensitive, accurate, specific and suitable for the quality control of the preparation.
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Objective To establish a method for determination of psoralen and isopsoralen in Bushen Jiannao Soft Capsule. Methods The HPLC separation was performed on Diamonsil-C18 (250 mm?4.6 mm, 5 ?m) column with a mixture methanol-water (48∶52) as the mobile phase, at a flow rate of 1.0 mL/min. Detection wavelength was at 246 nm, and column temperature at 40 ℃. Results The linear response of psoralen and isopsoralen ranged from 0.010 08～0.252 ?g (r=0.999 8) and 0.009 14～0.228 5 ?g (r =0.999 9). The average recovery was 98.91% (RSD=1.74%) and 99.93% (RSD=1.27%) respectively. Conclusion The method is simple, accurate, and suitable for the determination of the psoralen and isopsoralen in the preparations.
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Objective To establish a method for determination of puerarin in Yangwei Soft Capsule. Methods HPLC was used for quantitative ananlysis. The Phenomenex Kromasil C18 (250 mm?4.6 mm,5 ?m) column was used,and mobile phase was composed of methanol-water (22∶78). Detection wavelength was at 294 nm,the flow rate was 1.0 mL/min,column temperature was at 40 ℃,the injection volume was 10 ?L. Results The linear response ranges from 0.058 8～0.882 0 ?g of magnolol (r=0.999 9,n=6). The average recovery of magnolol is 99.35%,RSD=1.94%. The linear response ranges from 0.020 4～0.306 0 ?g of honokio (r =0.999 8,n =6). The averagy recovery of honokio is 99.21%,RSD=2.10%. Conclusion The method is simple,accurate,and suitable for the determination of the purarin in compound preparations.
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Object To study the formation of geoherbalism of Flos Lonicerae on the molecular level Methods Genomic DNAs from different populations of Lonicera japonica Thunb , outgroup Lonicera similis Hemsl , and Lonicera confusa DC were extracted, the 5S rRNA gene spacer region amplified, sequuenced, and analysed with Mega 1 02 Results The fragments of 5S rRNA gene spacer region in Lonicera L was about 210 bp with G+C content up to about 70% The sequences were different in various populations, and can be identified by sequencing The genetic distance between L confusa and L japonica was larger Conclusion The genuine distance between species was larger than that within species; the genetic distance among genuine crude drugs was smaller; the genetic distance among genuine and ungenuine crude drugs were bigger than that among genuine crude drugs