Determination of osthole in Jingyinling by gas chromatography - Master's thesis - Dissertation

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Determination of Osthole in Jingyinling by Gas Chromatography

Key words: Jingyinling, snake bedin, content determination, gas chromatography

Jingyinling is a kind of external preparation made by scientific processing of medicinal properties such as Cnidium, Sophora flavescens, Phellodendron chinense and white fresh skin.

,

It has the effects of clearing away heat and detoxifying, dehumidifying and relieving itching. Pharmacological experiments show that osthole in Cnidium is the main active ingredient in the treatment of vaginal trichomoniasis. This paper introduces the determination of osthole in Jingyinling by gas chromatography.

,

Simple method

,

Accurate results

,

Can be used as a net quality control indicator

,

In order to achieve the purpose of ensuring clinical efficacy.

1

Instruments, reagents and samples

Beijing Puri Analytical Instrument Co., Ltd.

GC-7800

Gas Chromatograph.

Osthole reference substance

:

China National Institute for the Control of Pharmaceutical and Biological Products

,

For the determination of content.

sample

:

Jiangxi Shangrao Pharmaceutical Factory

,

batch number

960524

,

940523

,

960526

.

2

Chromatographic conditions

Column

3mm × 200cm

Glass column

,

The body is

80

~

100

purpose

ChromosorbW (AWDMCS),

Stationary phase

5%

of

SE-30,

Column temperature

250 ° C,

Detector

FID,

Sensitivity

0.1,

Carrier gas is nitrogen

,

Flow rate is

30ml/min,

hydrogen

90kPa,

air

50kPa

.

3

Linear relationship

Accurately weigh the appropriate amount of osthole reference substance

,

Compatible

0.5mg/ml

Solution

,

Inject separately according to experimental conditions

1

,

2

,

3

,

4

,

5μl,

Gas chromatogram and corresponding peak area

,

Injection volume

(μg)

Plot the peak area integral value

,

Regression equation

:Y=2.63403 X ×0.000001+ 0.03673, r = 0.9998,

Linear range is

0.5

~

2.5mg/ml

.

4

Precision test

Precision extraction of osthole reference solution

(0.5mg/ml) 2μl,

Inject separately according to experimental conditions

5

Times

,

The relative deviation of the peak area value of the osthole reference substance is

1.2%

Indicates good precision.

5

Reproducibility experiment

Take this product

(

batch number

940524),

Repeat measurement by sample determination method

5

Times

,

Determination of osthole content

,

Relative standard deviation

1.8%,

Indicates good reproducibility.

6

Recovery test

Sample recovery method

,

Take a known amount of net yin

(

batch number

940524),

Precisely add osthole reference substance

,

Method according to sample content determination

,

Determination of content

,

Calculate recovery

,

Average recovery

97.1%

Relative standard deviation

2.1%

.

7

Sample determination

Precise measurement

50ml,

In the separatory funnel

,

With extraction

5

Times

,

Each

50ml,

Combined extract

,

Dehydrated with anhydrous sodium sulfate

,

Filtrate

,

Filtration with a small amount of washing

,

Combine filtrate and lotion

,

Low temperature evaporation with a rotary evaporator

,

Residue added to dissolve

,

Tolerance

2ml

In the bottle

,

As a test solution

,

Injection

2μl

analysis.

8

discuss

use

5% SE-30

Analysis of osthole in samples for stationary phase packed columns

,

The chromatographic peak of osthole can reach baseline separation

,

It is equivalent to the separation effect of the quartz capillary column reported in the literature.