Hirsutella sinensis mycelium powder capsules, a new unique health product, is mainly composed of hirsutella sinensis mycelium powder which is separated from natural cordyceps sinensis.Compared with natural cordyceps sinensis, this Capsule has the same health functions while its price is only one-thirtieth of it. So the capsule is gradually replacing natural cordyceps sinensis and the market demand of it is increasing fast. But different from the medicine market which is well supervised, the health product market is highly chaos and has many kinds of health products that they have distinctive nature of characteristics. Moreover, there are no appropriate quality standards for hirsutella sinensis mycelium powder capsules. So it is urgent for us to establish appropriate quality standards for it to control the stablities of technology and quality and protect the health and rights of consumers.ObjectiveEstablish the fingerprint of hirsutella sinensis mycelium powder capsules by using high performance liquid chromatography and X-ray powder diffraction and research the fast separation and determination methods of functional composition. Through these methods, controlling the technology and quality stablities of the capsules is our final aim.Methods1 Establish the fingerprint by using high performance liquid chromatography, use ultra-pure water as solvent, ultrasonic extrat in 50℃for 90min, use 0.04mol/L potassium dihydrogen phosphate solution-acetonitrile as mobile phase gradient elution, Hypersil BOS C18(4.6mm×250mm,5μm) column,260nm wavelength detection, HPLC-PDA method.2 Acquire XRD fingerprint of ten batches hirsutella sinensis mycelium powder capsules. Compare to different kinds of products with optimized XRD instrument parameters. With Japan Rigaku MiniFlexâ…¡X-ray powder diffraction, CuMo radiation, graphite monochromator, tube voltage 30 kV, tube current 15 mA,2θscanning range 5°~55 ,scanning speed 5°/min, step length 0.02°, divergence slit 1.25°, receiving slit 0.3 mm, anti-scatter slit 1.25°.3 With 95% ethanol solvent, ultrasonic extraction in 80℃for 90min, methanol as mobile phase, UltimateTM AQ-C18(4.6×250mm,5/μm) column, 1.0mL/min flow rate, column temperature is 30℃,10μL injection volume,282nm wavelength detection, Detect the free ergosterol in hirsutella sinensis mycelium powder capsules by HPLC-PDA.Results1 Established the unique nucleotides which is reference substance components fingerprint of hirsutella sinensis mycelium powder capsules by HPLC. Selected 19 characteristic common peaks, the similarity of S1~S10 were between 0.974 to 0.988, all are above 0.900.2 Established the unique fingerprint of hirsutella sinensis mycelium powder capsules by X-ray powder diffraction. Selected 7 characteristic common peaks by origin 7.5 software.The correlation coefficients of S1~S10 were all above 0.9950 and the similar coefficient of vector angular cosine were all above 0.9996. The macroscopical trend of XRD fingerprint among artificial cordyceps militarisã€yuankang capsules and hirsutella sinensis mycelium powder capsules was similar, but their characteristic peaks were different.3 Established the most appropriate method to extract and separate free ergosterol in hirsutella sinensis mycelium powder capsules and to determine its concentration by HPLC. The average content of three different batches wasl.6489ã€1.6858ã€1.5827mg·g-1, The contents were fitted for fine linear correlation during the circumscription of 18.0~180.0μg·mL-1 by HPLC(r=0.999), Detection limits was 340ng·mL-1(SNR=3.0).The range of the spotting recovery rate was 100.45%.Conclusions1 The fingerprint of nucleotides components in hirsutella sinensis mycelium powder capsules by HPLC was well exclusive and repeatable, which can reflect the stablity of technology and quality of this product and provide reliable informations for the quality certification.2 The fingerprint of hirsutella sinensis mycelium powder capsules by XRD was well exclusive and abundant. It can evaluate stablity and identify different kinds of products. It made use of and developed new ideas of XRD.detective to control the quality of health foods and indentify the different health products.3 The method of free ergosterol determination by HPLC was simple and fast. It has highly repeatability and selectivity, which can satisfy the needs of routine testing. |