Jingfukang Pharmaceutical Group Co Ltd.

The quality standards of the new medicine Chaiqin Soft Capsule were established.Radix Bupleuri, Radix Puerariae, Radix Sophorae Tonkinensis and Rhizoma Cimicifugae were identified by TLC.And the content of baicalin in Scutellaria baicalensis was determined by HPLC.The HPLC system was with Diamonsil C₁₈ (250 mm × 4.6 mm, 5 μm) column, the mobile phase was methanol-water-phosphoric acid (47:53:0.2), flowing rate was 1.0 mL/min, UV detecting wavelength was at 280 nm, and the column temperature were at 20°C.The test product, the reference drug and the reference standard chromatog. had the same color of the spots in the corresponding position but the neg. sample excepted.The study on the quality control showed that the characteristics of identification by TLC was distinct and highly specific.Baicalin showed a good linear relationship at a range of 0.28-1.40 μg (r=0.9999), the average recovery was 99.74%, and RSD was 0.85%.The method could effectively control the quality of products.

Objective To explore the optimal extraction process of volatile oil in Angelica sinensis, Notopterygium incisum, and Radix saposhnikoviae from Huoxue Runchang Soft Capsules by steam distillationMethods Orthogonal exptl. design was used to evaluate the extraction rate.The influence of the amount of water, soaking time, extraction time and the amount of salt added on the extraction rate of volatile oil was investigated.The chem. composition of the volatile oil was analyzed by gas chromatog.-mass spectrometry( GC-MS).Results The optimal extraction process was adding 6 times the amount of water, soaking for 1.5 h, and extracting for 4 h.Under these conditions, the extraction rate of the volatile oil was 0.34%; the main component obtained by GC-MS anal. was 1, 4-double( 1-methylethyl)-benzene, 1 R-α-pinene, β-pinene, furan acetate, ( R)-4-methyl-1-( 1-methylethyl)-3-cyclohexene-1-alc., limonene, etc.Conclusion Soaking time, water addition and extraction time have no significant influence on the extraction rate of volatile oil.The order of influence is soaking time > water addition > extraction time.

Objective To establish a method for the determination of testosterone in deer blood by solid phase extraction coupled with liquid chromatog.-mass spectrometry for the quality control of deer blood.Methods Firstly, the samples were pretreated, and then the testosterone content in deer blood was determined by using fixed quantum ion(109.06) under the conditions of liquid chromatog. and mass spectrometry.Build sample preparation: acetonitrile precipitation deer blood protein, Et acetate extracted first testosterone, the solution to the activation of SAX(Maximum loading volume was 500 mg, volume was 3 mL) solid phase extraction column, the liquid obtained by nitrogen blow to nearly dry, N-hexane extraction, three times to add to the activated Florisil(maximum loading volume was 500 mg, volume was 3 m L) solid phase extraction column, abandon the filtrate, Et acetate, N-hexane(60:40, V/V) elution pillars, nitrogen blow dry.The solution was dissolved in 50% methanol and passed through 0.22 μm microporous filtration membrane.High performance liquid chromatog. condition: shim-Pack XR-ODS column(2.0 mmx75 mm, 2.2 μm).The mobile phase consisted of methanol-0.1% formic acid-water and gradient elution.Column temperature was 40°C.Flow rate was 0.3 m L/min.Sample size was 20 μL.The mass spectrum condition: de-clustering voltage(DP) was 60.0 V, collision energy(CE) was 10.0 e V.Results In the linear range of 1.5165x10∼(-4) to 3.033x10∼(-1)μg/mL, the R of the fixed quantum ion 109.06 was 0.9995.The average recovery was 66.62%(n=6), RSD was 3.44%.The content of testosterone in four batches of deer blood was 3.30x10∼(-4) to 3.48x10∼(-4)μg/mL, with RSD <3%.Conclusion The method for the determination of testosterone in deer blood by solid phase extraction coupled with liquid chromatog.-mass spectrometry was established.The linear range and recovery rate of solid phase extraction coupled with liquid chromatog.-mass spectrometry are in line with the requirements of laws and regulations, and could provide reference for the quality evaluation of deer blood.