Determination of osthole by gas chromatography

Bedidin is one of the anti-bacterial antipruritic, treatment of vaginal trichomoniasis white fresh skin and other medicinal taste, according to the experimental conditions were injected 1, 2, 3, 4, ChromosorbW (AWDMCS), the stationary phase is 5% SE-30, column temperature 250 ℃, detector FID, sensitivity 0.1, carrier gas nitrogen, flow rate 30ml / min, hydrogen 90kPa, air 50kPa. 3l) 2μl, respectively inject 5 ~ 2.5mg / ml according to the experimental conditions.

Appropriate amount of fine reference substance, formulated into 0.5mg / ml chloroform solution. Keywords: Jingyinling, osthole, content determination, gas chromatography density test, precision absorption of osthole reference substance solution (0.5mg / m min. This article introduces gas phase Chromatographic determination of the content of osthole in Jingyinling is simple and accurate, and can be used as the internal quality control index of Jingyinling, to ensure that the guarantee is 5μl, and the gas chromatogram and corresponding peak area are obtained by injection volume (μg ) The integral value of the peak area is plotted, and the regression equation is obtained: Y = 2.63403 X × 0.000001 + 0.03673, r = 0.9998, linear range is 0.5 gas chromatography column 3mm × 200cm glass column, and the support is made by scientific processing of 80 ~ 100 mesh An external preparation, has the effect of clearing heat and detoxification, dehumidification and itching. Pharmacological experiments show the purpose of the curative effect of the snake bed.
1 Instrument 960524, 940523, 960526.
2 Chromatographic conditions, the relative deviation of the peak area value of the osthole reference is 1.2%, indicating good precision.

Reproducibility experiment Take this product (batch number 940524) and repeat the measurement 5 times according to the sample measurement method, respectively, and determine the content of osthole, the relative standard deviation is 1.8%, indicating good reproducibility.

Recover rate tester, try to measure the amount of Jingyin Ling 50ml, place in a separating funnel, extract 5 times with chloroform, 50ml each time, combine chloroform extracts, dehydrate with anhydrous sodium sulfate, filter out chloroform solution, filter hawthorn Wash with a small amount of chloroform, combine the filtrate and the washing liquid, use a rotary evaporator to use the sample recovery method, take a packed column with a known content of% SE-30 as the stationary phase, and analyze the osthole in the sample. The peak can reach the baseline dose and sample. The GC-14B gas chromatograph and CR-6A data processor produced by Shimadzu Corporation of Japan.

Ophiopogon reference substance: provided by China National Institute for the Control of Pharmaceutical and Biological Products, used for content determination.
Sample: Produced by Shangrao Pharmaceutical Factory, Jiangxi Province, batch number

Edited by Ke Mingqing, Physicochemical and pharmacological properties of active ingredients of Chinese herbal medicine, Changsha: Hunan Science and Technology Press, 1979.261

Gao Hai, Journal of Pharmaceutical Analysis, 1991, 11 (6): 361
Jingyinling (Lot No. 940524) was added with the osthole reference substance, the content was determined according to the method of sample content determination, and the recovery rate was calculated. The average recovery rate was 97.1% and the relative standard deviation was 2.1%.

The main effect of the sample to determine the disease is a linear relationship. The osthole is accurately weighed and evaporated, and the residue is dissolved by adding chloroform. The volume is fixed in a 2ml measuring flask and used as the test solution. Inject 2μl for analysis.
discuss

Jingyinling is composed of snake bed, Sophora flavescens, Phellodendron chinense,
The fine separation is equivalent to the separation effect reported by the quartz capillary column in the literature.
Reference Wen 5

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