QB/T 2966-2014Functional toothpastes (English PDF)

4.1 Raw material

The raw materials used in the production of functional toothpaste shall meet the requirements of GB 22115.

4.2 Hygiene indicators

The hygiene indicators shall be in accordance with GB 8372.

4.3 Sensory, physical and chemical indicators

Sensory, physical and chemical indicators are in accordance with GB 8372.

4.4 Efficacy evaluation and safety requirements

a) The efficacy evaluation study shall be conducted on the basis of the safety evaluation of the functional components;

b) The efficacy involved in WS/T 326 is performed according to the evaluation method of WS/T 326;

c) Toothpaste products that claim to have same efficacy, use the same functional components, and have an added amount not less than the proved, do not need efficacy evaluation;

d) For the efficacy evaluation report (including clinical evaluation report and laboratory evaluation report), at least one shall be issued by the institution that meets one of the following qualifications:

1) Grade III Class A oral medical institutions (including the School of

Stomatology, Stomatological Specialty Hospitals and General Hospital

Stomatological Departments) with the qualification of "Pharmaceutical

Clinical Trial Institute" of the State Food and Drug Administration (SFDA). If it is a stomatology department of a general hospital, it must have had the stomatology qualification certificate of "Drug Clinical Trial

Agency";

2) School of stomatology / specialized hospital, awarded by the Ministry of Health as a key clinical specialty (stomatology);

3) Provincial stomatological hospital (the project leader must have passed the national drug clinical trial technical training and passed the assessment, and obtained the GCP certificate).

e) The laboratory evaluation report can also be issued by a national or provincial third-party laboratory organization whose qualification is qualified.

5.4 Safety

In order to ensure the safety of the product, the components added in the functional toothpaste shall meet the requirements of GB 22115.

5.5 Qualitative or quantitative determination of functional components

The enterprise tests the functional components according to the measurement method (recommended but not limited to) described in the annex of this

Standard. It can also issue a report after being detected by a domestic third- party testing agency. If there are other functional components and their determination methods, they shall be supplemented and perfected in the in accordance with WS/T 326. There is currently no prescribed method for efficacy evaluation, which shall be conducted in accordance with the principles prescribed in this Standard.

Annex B (informative)

Determination of paeonol content

B.1 Instrument

High performance liquid chromatography.

B.2 Reagents

B.2.1 Paeonol reference substance (China National Institute for the Control of

Pharmaceutical and Biological Products).

B.2.2 Methanol: chromatographically pure.

B.3 Preparation of reference substance solution

Weigh 0.01g of paeonol reference substance (to the nearest of 0.0001g) in a volumetric flask. Add methanol to dissolve and make 0.032mg/mL paeonol solution.

B.4 Preparation of sample solution

Weigh 0.2g of sample (to the nearest of 0.0001g) in a stoppered test tube.

Accurately add 10mLof methanol. Use a glass rod to stir the toothpaste sample.

Conduct ultrasonic extraction 30min. Place still. Pour the supernatant into a centrifuge tube. Centrifuge at 2000r/min for 5min. Use a 0.45µm filterable membrane to filter and the solution shall be obtained.

B.5 Determination

B.5.1 Chromatographic conditions

Chromatographic column: C 18 250mm×4.6mm, 5µm.

Mobile phase: methanol + water (73+27).

Flow rate: 1mL/min.

Detector: UV detector with a wavelength of 274nm.

Column temperature: 40°C.

B.5.2 Reference substance solution

Annex C (informative)

Determination of potassium content

C.1 Reagents a) Hydrofluoric acid;

b) Hydrochloric acid c) Nitric acid;

d) Nitric acid solution: (1+1);

e) Nitric acid: 1%;

f) Hydrogen peroxide: 30%;

g) Dissolved acetylene: meet requirements of GB 6819-2004;

h) Potassium standard stock solution: Accurately weigh 1.9068g of potassium chloride that has been burnt at 500°C~600°C to constant weight. Dissolve in water. Dilute to 1000mL. Potassium concentration is

1000mg/L. When it is used, dilute it to 100mg/L potassium standard stock solution.

C.2 Instruments a) Atomic absorption spectrophotometer: wavelength is 769.9nm;

b) Potassium hollow cathode lamp;

c) Electronic balance: resolution is 0.0001g.

C.3 Preparation of sample solution

Randomly take 1 sample toothpaste. Discard about 20mm paste of head.

Weigh 0.25g of toothpaste sample (to the nearest of 0.0001g) in a 50mL beaker.

Add 1.5mL of hydrochloric acid. Add 4.5mL of (1+1) nitric acid to dissolve. Add

5 drops of 30% hydrogen peroxide. Heat to slightly boiling. If red-brown gas appears during the digestion process, continue to add a small amount of dilute nitric acid for digestion. Heat till it is nearly dried. Then use 1% nitric acid solution to set volume into a 50mL volumetric flask. Shake well for testing. At the same time, conduct blank test.

Annex E (informative)

Determination of saponins in Panax notoginseng (Tianqi)

E.1 Instruments a) High performance liquid chromatograph: equipped with ultraviolet detector;

b) Micro-sampler: 20µL;

c) Ultrasonic cleaning machine;

d) Electronic balance: resolution is 0.0001g.

E.2 Reagents a) Ginsenoside Rg 1 reference substance (China National Institute for the

Control of Pharmaceutical and Biological Products);

b) Ginsenoside Rb1 reference substance (China National Institute for the

Control of Pharmaceutical and Biological Products);

c) Notoginsenoside R 1 reference substance (China National Institute for the

Control of Pharmaceutical and Biological Products);

e) Methanol: chromatographically pure; [Translator: d) is missing in original text] f) Acetonitrile: chromatographically pure.

E.3 Preparation of reference substance solution

Respectively weigh the right amount of ginsenoside Rg1 , ginsenoside Rb1 and notoginsenoside R 1 reference substances (to the nearest of 0.0001g). Add methanol to make a mixed solution containing 0.1mg of each reference substance per 1mL as the reference substance solution.

E.4 Preparation of sample solution

Randomly take a sample toothpaste. Discard 20mm~30mm paste of head.

Weigh 4.5g of toothpaste sample (to the nearest of 0.0001g) in a 150mL beaker.

Add 10mL of water. Slightly heat and use a glass rod to stir, making it completely dissolve. Add methanol solution to 100mL. Weigh the mass. Conduct ultrasonic extraction 30min. Take it out. Place still till it is cool. Then weigh the mass again.

Use methanol to make up for the lost mass. Shake well. Filter. Take the filtrate

F.3.7 Chloroform.

F.3.7 Ethyl sulfate solution (1->10). [Translator note: F.3.7 is repeated in original text]

F.3.8 Ginsenoside R g1 standard product (China National Institute for the Control of Pharmaceutical and Biological Products).

F.3.9 Notoginsenoside R 1 standard product (China National Institute for the

Control of Pharmaceutical and Biological Products).

F.4 Sample preparation and determination

F.4.1 Preparation of tested sample solution

Weigh 25g of toothpaste in a 100mL Erlenmeyer flask. Add 60mL of 95% ethanol. Stir well. Conduct ultrasound 30min. Perform supernatant filtration.

Respectively use 30mL, 20mLof 95% ethanol to wash the filter residue.

Combine the filtrate in an evaporating dish. Concentrate to thick material on a

90°C water bath. Add 30mL of water to dissolve the thick material and transfer to a separatory funnel. Use petroleum ether (boiling range is 60°C~90°C) to extract 3 times, 20mL for each time. Discard the petroleum ether layer. Use water-saturated n-butanol to extract the aqueous layer for 3 times. The amount of water-saturated n-butanol is 50mL, 25mL, 25mL, respectively. Discard the aqueous layer. The n-butanol layer is placed in an evaporating dish and evaporated to dryness on a 90°C water bath. Add 8mL of water to dissolve the residue (can be heated at 30°C to promote dissolution). Neutral alumina column is on aqueous solution (inner diameter is 17mm, length is 50mm). Use 100mL of NaOH solution (that is, 0.1mol/L->20) of which the pH is 10~10.5. 500mL of pure water, 50mL of 30% ethanol to elute in turn. Collect 30% ethanol eluent and place in evaporating dish. Evaporate on the 90°C water bath. Add 1mL of methanol to dissolve the residue as the tested product solution.

F.4.2 Preparation of standard solution

Take ginsenoside Rg 1 reference substance, notoginsenoside R 1 reference substance. Respectively add methanol to make the solution that each 1mL contains 0.5mg, as the reference substance solution.

F.4.3 Determination

Test according to "Chinese Pharmacopoeia" (Edition 2005) (Annex VI B) "Thin

Layer Chromatography". Respectively pipette 10µL of above three solutions.

Respectively drop on the same silicone G thin layer board. Use chloroform- methanol-water (7: 3: 0.5) as the developing agent. Unfold, take out and dry.

Spray with sulfuric acid and ethanol solution (1->10). Heat at 105°C until the spots are clear. In the chromatogram of the test product, the spots of the same

Annex G (informative)

Determination of active component of grass coral

G.1 Reagents a) Methanol;

b) Chloroform;

c) Standard isopyridine stock solution: Take 0.008g of isopyridine reference substance (to the nearest of 0.0001g). Add methanol to dissolve and prepare a standard solution containing 4µg per 1mL.

G.2 Instruments a) High performance liquid chromatograph: wavelength is 344nm;

b) Ultrasonic cleaning machine;

c) Electronic balance: resolution is 0.0001g.

G.3 Preparation of sample solution

Table about 10g of sample (to the nearest of 0.0001g). Place in a 100mL stopper Erlenmeyer flask. Precisely add 50mL of water. Weigh the mass.

Conduct ultrasonic treatment 30min. Stand overnight. Then conduct ultrasonic treatment 30min (power is 300W, frequency is 25kHa). Take it out. Cool to room temperature. Make up for the mass. Shake well. Filter. Precisely measure 25mL of filtrate. Transfer to the separating funnel. Use chloroform to extract 3 times,

20mL each time. Combine chloroform extracts. Heat to evaporate till dry. Add methanol to dissolve the residue and move into a 25mL volumetric flask. Add methanol to the scale. Shake well for spectrum analysis. At the same time, conduct blank test.

G.4 Determination

G.4.1 Instrument conditions

Chromatographic column: C 18 250mm×4.6mm, 5µm.

Mobile phase: acetonitrile-0.1% phosphoric acid solution (20:80).

Flow rate: 1 mL/min.