金银花的质量标准控制(个人向)
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Drug Standards of Quality Control of
Lonicerae Japonicae Flos
14402020林程
Objectives
1.Master the microscopic identification of LJF.
2.Master the description of LJF and learn the difference of description between LJF and LF.
3.Master the TLC identification of LJF and LF.
4.Master the method for the determination of marker constituents in crude drug.
5.Study the application of HPLC in determination of chlorogenic acid and luteolin-7-O-glucoside in LJF.
Methods
(I).Identifications
1.Description
Breed LFJ LF
Character Clavate,stout in upper part and
tapered downwards,slightly curved
Clavate,slightly curved
Surface color Yellow white or green white Green Brown to yellow white
Size2~3cm long,upper diameter is3mm,
downwards diameter is1.5mm 3~4.5cm long,upper diameter is2mm, downwards diameter is1mm
Wistiti Densely Less
2.Microscopic identification
i).Preparation of slides of corolla surface.
Tear LJF corolla by tweezers————→Place LJF corolla on the slide————→Add1-2 drops of glycerine alcohol mixture and put the cover on the slide
ii).Preparation of slides of LJF powder
Place small amount of powder on the slide————→Add1-3drops of chloral hydrate————→Heat and stir by alcohol lamp————→Absorb the excess liquid by paper————→Use forceps to put the cover on the slide by one side————→Add1-2drops of glycerine alcohol mixture
iii).Observe characteristics of LJF
Glandular hairs
·The head of glandular hairs are multicellular with subrounded or slightly oblate.
·The stalks of glandular hairs are unicellular or multicellular.
Non-glandular hairs
•Numerous.
•Thick walls,unicellular,with fine verrucae on the surface,some have corneous spiral.•Thin walls,slender,curved or shrinkage,with fine verrucae on the surface.
Pollen grains
·Pollen grains are spherical,with3germinal pores.
3.TLC identification of LJF and LF
i).Differences of morphological between LFJ and LF
Breed LFJ LF
Organic acids+
Chlorogenic acid
+ Chlorogenic acid
Flavonoids++ Iridoids++ Saponins-+
Macranthoidin B
Dipsacoside B
ii).Experiment Materials
•TLC silica gel plate(10cm×5cm),chromatography cylinder,capillary tube
•Developing solvent:mixture of n-butanol,formic acid and water(4:1:5)
•Reference substances:Macranthoidin B(5mg/ml),Dipsacoside B(5mg/ml),Chlorogenic acid(1mg/ml)
•Chromogenic agent:10%sulfuric acid in ethanol(saponins chromogenic agent)
•Samples:powder of LJF and LF
TLC procedures
•Sample solution preparation:Add1g powder of LJF and LF into10ml methanol, sonicated for about10minutes,filter,and get supernatant as sample solution.
•Chromatography cylinder saturation:Add developing solvent into the chromatography cylinder,saturated.
•Spotting:Add reference substances(chlorogenic acid,dipsacoside B,macranthoidin B),LJF, LF.Put the plate into the chromatography cylinder,cover the lid.
•Developing Distance:5~6cm
•Examination:1.Observe the spot under UV light at365nm(chlorogenic acid).2.Spray with10%sulfuric acid in ethanol,heat at105ºC for1~2min and observe under daylight (saponins).
iii).Ideal result
1:chlorogenic acid
2:Macranthoidin B
3:Dipsacoside B
4:LF sample solution
5:LFJ sample solution