金银花

English text reference: *Chinese Pharmacopoeia (2020 Edition) *

Overview

Honeysuckle Flower is the dried flower bud or the flower with the initial opening of Lonicera japonica Thunb. (Fam. Caprifoliaceae). The drug is collected in early summer before the flowers open and dried.

Description

Flower buds are cylindrical, upper part thick and lower part thin, slightly curved, 2-3 cm long, upper part about 3 mm in diameter, lower part about 1.5 mm in diameter; surface yellowish-white or greenish-white (becoming darker on storage), densely covered with short, soft hairs; occasionally with leaf-like bracts. Calyx green, 5-lobed at apex, lobes hairy, about 2 mm long. Corolla tubular, 2-lipped at apex; stamens 5, adnate to corolla tube, yellow; ovary glabrous. Odour, fragrant; taste, mild and slightly bitter.

Identification

（1）The powder is light yellowish-brown or yellowish-green. There are more glandular hairs, with the head inverted conical, circular or slightly flattened, consisting of 4-33 cells, arranged in 2-4 layers, with a diameter of 30-64-108 μm, and the stalk consisting of 1-5 cells, up to 700 μm long. There are two types of non-glandular hairs: one is thick-walled non-glandular hairs, single-celled, up to 900 μm long, with micro-papillary or vesicular protrusions on the surface, some with spiral patterns; the other is thin-walled non-glandular hairs, single-celled, very long, curved or wrinkled, with micro-papillary protrusions on the surface. The diameter of calcium oxalate cluster crystal is 6-45 μm. Pollen grains are round or triangular, with fine short spines and granular sculptures on the surface and have 3 colpi.

（2）Take 0.2 g of the powder, add 5 ml of methanol, let it stand for 12 hours, filter, and take the filtrate as the test solution. Take chlorogenic acid reference substance, add methanol to make a solution containing 1 mg per ml as the reference solution. Carry out the method for thin layer chromatography <0502>, using silica gel H as the coating substance and the upper layer solution of ethyl acetate-butanoic acid-water (7: 2.5: 2.5) as the mobile phase. Apply separately to the plate 10-20 μl of the test solution and 10 μl of the reference solution. After developing and removal of the plate, dry in air. Examine under ultraviolet light at 365 nm. The fluorescent spot in the chromatogram obtained with the test solution corresponds in position and colour to the spot in the chromatogram obtained with the reference solution.

Characteristic mapping

Determined by high performance liquid chromatography <0512>.

Chromatographic conditions and system suitability test

Same as under [Content Determination] Phenolic Acids except that the detection wavelength is 240 nm.

Preparation of reference solutions

Take the appropriate amount of chlorogenic acid control product, precision weighing, add methanol to make a solution containing 0.40 mg per ml, that is to obtain.

Preparation of test solution

Same as under [Content Determination] Phenolic Acids.

Determination method

Precisely aspirate 2 μl each of the reference solution and the test solution respectively, inject into liquid chromatograph and determine, it is obtained.

The characteristic profile of the test product should show seven characteristic peaks, and the peak corresponding to the reference peak is the S peak, calculate the relative retention time of each characteristic peak and the S peak, which should be within ±10% of the specified value, the retention time specified values are: 0.91 (peak 1), 1.00 [peak 2 (S)], 1.17 (peak 3), 1.38 (peak 4), 2.43 (peak 5), 2.81 (peak 6), 2.93 (Peak 7).

Examination

Water

Not more than 12.0 per cent <0832, method 4>.

Total ash

Not more than 10.0 per cent <2302>.

Acid-insoluble ash

Not more than 3.0 per cent <2302>.

Heavy metals and harmful elements

Determined by the method of lead, cadmium, arsenic, mercury, and copper (atomic absorption spectrophotometry or inductively coupled plasma mass spectrometry) <2321>. The limit of lead is not more than 5 mg/kg; the limit of cadmium is not more than 1 mg/kg; the limit of arsenic is not more than 2 mg/kg; the limit of mercury is not more than 0.2 mg/kg; the limit of copper is not more than 20 mg/kg.

Assay

Phenolic acids

Determined by high performance liquid chromatography <0512>.

Chromatographic conditions and system suitability test

Octadecylsilane-bonded silica gel was used as filler; acetonitrile was used as mobile phase A and 0.1% phosphoric acid solution was used as mobile phase B. The gradient elution was carried out according to the following table; the temperature of the column was not higher than 25 ℃; the flow rate was 0.7 ml per minute, and the detection wavelength was 327 nm. the number of theoretical plates should be not less than 10,000 according to the calculation of chlorogenic acid peak.

Preparation of reference solution

Take chlorogenic acid control, 3,5-di-O-caffeoylquinic acid control and 4,5-di-O-caffeoylquinic acid control in appropriate amount, weighed accurately, placed in a brown measuring flask, and added with 75% methanol to make a solution containing 0.28 mg, 0.15 mg, and 44 μg per ml, that is, obtained.

Preparation of test solution

Take the powder of this product (through the fourth sieve) about 0.5 g, precision weighing, placed in a stoppered conical flask, precision addition of 75% methanol 50 ml, weighing, ultrasonic treatment (power 500 W, frequency 40 kHz) for 30 minutes, cooled, and then weighing, 75% methanol to make up for the loss of weight, shaking, filtration, and take the filtrate, that is, the product is obtained.

Determination method

Pipette 2 μl each of control solution and test solution, inject into liquid chromatograph, and then determine, that is, obtain.

This product contains not less than 1.5% chlorogenic acid (C16H18O9) calculated as dried product, and not less than 3.8% phenolic acids calculated as the total amount of chlorogenic acid (C16H18O9), 3,5-di-O-caffeoylquinic acid (C25H24O12) and 4,5-di-O-caffeoylquinic acid (C25H24O12).

Luteoloside

Determined by high performance liquid chromatography <0512>.

Chromatographic conditions and system suitability test

Phenylsilane bonded silica gel was used as filler (Agilent ZORBAX SB-phenyl 4.6 mm×250 mm, 5 μm), with acetonitrile as mobile phase A and 0.5% glacial acetic acid solution as mobile phase B. Gradient elution was carried out in accordance with the following table; the detection wavelength was 350 nm. the theoretical plate counts calculated on the basis of the lignoceroside peaks should be not less than 20,000.

Preparation of reference solution

Take the appropriate amount of lignocaine control, precision weighing, add 70% ethanol to make a solution containing 40 μg per ml, that is to obtain.

Preparation of test solution

Take this product powder (through the fourth sieve) about 2 g, precision weighing, placed in a stoppered conical flask, precision addition of 70% ethanol 50 ml, weighing, ultrasonic treatment (power 250 W, frequency 35 kHz) for 1 hour, cooling, and then weighing, with 70% ethanol to make up for the loss of weight, shaking well, filtered. Precisely measure 10 ml of the filtrate, recover the solvent to dry, the residue was dissolved with 70% ethanol, transferred to a 5 ml measuring flask, add 70% ethanol to the scale, that is, obtained.

Determination method

Pipette 10 μl each of control solution and test solution, injected into liquid chromatograph, and then measured, it is obtained.

This product contains not less than 0.050% of lignocaine (C21H20O11) calculated as dried product.

Property

Cold.

Flavor

Sweet.

Meridian tropism

Lung, heart, and stomach meridians.

Actions and Indications

To clear heat and detoxify and disperse wind-heat.

Indications

Used for carbuncles and sores, sore throat, erysipelas, dysentery due to heat-toxin, wind-heat common cold, and febrile diseases.

Dosage

6-15 g.

Administration

None.

Storage

Preserve in a cool and dry place, moisture-proof, and mothproof.

金银花

Text reference: Chinese Pharmacopoeia (2015 Edition)

Overview

Honeysuckle Flower is the dried flower bud or opening flower of Lonicera japonica Thunb. (Fam Capri-foliaceae ). The drug is collected before flowering in early summer, and dried.

Description

Clavate, stout in upper part and tapered downwards, slightly curved, 2-3 cm long, about 3 mm in diameter in upper part and 1.5 mm in diameter in lower part. Externally yellowish-white or greenish-white, gradually darken on keeping, densely pubescent. Foliaceous bracts occasionally visible. Calyx green, 5-lobed at the apex, lobes pubescent, about 2 mm long. Corolla tubular when open, apex 2-lipped, stamens 5. epipetalous, yellow; pistil 1, ovary glabrous. Odour, delicately aromatic; taste, weak and slightly bitter.

Identification

（2）取本品粉末0.2g，加甲醇5ml，放置12小时，滤过，取滤液作为供试品溶液。另取绿原酸对照品，加甲醇制成每1ml含1mg的溶液，作为对照品溶液。照薄层色谱法（通则0502） 试验，吸取供试品溶液10～20µl、对照品溶液10µl，分别点于同一硅胶H薄层板上，以乙酸丁酯-甲酸-水（7：2.5：2.5）的上层溶液为展开剂，展开，取出，晾干，置紫外光灯（365nm）下检视。供试品色谱中，在与对照品色谱相应的位置上，显相同颜色的荧光斑点。

Examination

Water

Not more than 12.0 per cent <0832, method>.

Total ash

Not more than 10.0 per cent <2302>.

Acid-insoluble ash

Not more than 3.0 per cent <2302>.

Heavy metals and harmful elements

Carry out the method for determination of lead, cadmium, arsenic, mercury and copper <2321,atomic absorption spectrophctometry, or inductively coupled plasma mass spectrometry>, not more than 20 mg/kg of lead. 0.3 mg/kg of cadmium, 2 mg/kg of arsenic, 0.2 mg/ kg of mercury and 20 mg/kg of copper.

Assay

Chlorogenic acid

Chromatographic system and system suitability Use octadecylsilane bonded silica gel as the stationary phase and a mixture of acetonitrile and 0.4% phosphoric acid solution (13 : 87) as the mobile phase. As detector a spectrophotometer set at 327 nm. The number of theoretical plates of the column is not less than 1000, calculated with reference to the peak of chlorogenic acid.

Luteolin-7-0-glucoside

Chromatographic system and system suitability Use phenyl silane bonded silica gel as the stationary phase, acetonitrile as the mobile phase A, 0.5% glacial acetic acid solution as the mobile phase B, elute in gradient as the following:

(min) Mobile phase A

Reference solution Dissolve a quantity of luteolin-7-O- glucoside CRS, accurately weighed, in 70% ethanol to produce a solution of 40 μg per ml as the test solution.

Property and Flavor

Cold, sweet. Meridian tropism Lung, heart and stomach meridians.

Actions and Indications

To clear beat, remove toxin, and disperse wind- beat. Indications Swelling abscess, deep-rooted boil, sore, throat bi disorder, erysipelas, heat-toxin blood dysentery, common cold caused by wind-heat, and fever in warm disease.

Administration and dosage

6-15 g.

Storage

Preserve in a cool and dry place, and protect from moisture and moth.