YY/T 0823-2020Fluoride compounds used for dental carious prevention (English PDF)

3.1 Soluble fluoride

Fluorine, of soluble fluoride compounds used for dental carious prevention, which is soluble in water. deviation of the total fluorine content from the package nominal value shall not exceed ±20 % of the package nominal value.

5.4 Total content of heavy metals (in terms of Pb)

Test according to the method of 7.5, the total content of heavy metals (in terms of Pb) of the sample shall be less than 20 mg/kg.

5.5 Arsenic content

Test according to the method of 7.6, the arsenic content of the sample shall be less than 5 mg/kg.

5.6 Microbial limit (applicable to water-soluble type products)

5.6.1 Total number of aerobic bacteria: not more than 102 CFU/g or not more than 102 CFU/mL.

5.6.2 Total number of molds and yeasts: not more than 101 CFU/g or not more than 101 CFU/mL.

5.6.3 Pseudomonas aeruginosa: not detectable.

5.6.4 Staphylococcus aureus: not detectable.

5.6.5 Escherichia coli: not detectable.

NOTE: 101 CFU: indicates that the maximum acceptable number of bacteria is 20.

102 CFU: indicates that the maximum acceptable bacterial count is 200.

7.1 General

All tests shall be carried out under the conditions of temperature (23 ± 2) °C and humidity (50 ± 5) %, unless otherwise specified. If the material is stored under refrigeration, it shall be placed in the test environment at least 4 h in advance.

7.2.3 Result determination

The result determination is as follows:

a) Take two samples for each product. If the two results both comply with the provisions of 5.1, then it meets the requirements of the standard.

b) If one of the two results does comply with the provisions of 5.1, take three new samples and test again. If the three results all comply with the provisions of 5.1, the item meets the requirements of this Standard, otherwise it does not meet the requirements of this Standard.

7.3 Soluble fluorine content

7.3.1 Calibration working curve

7.3.1.1 Total ionic strength adjustment buffer (TISAB II).

7.3.1.3 Standard solutions: 0.1 µg/mL, 0.5 µg/mL, 1 µg/mL, 5 µg/mL, 10 µg/mL, 20 µg/mL, 50 µg/mL.

7.3.1.4 According to the equipment and test methods required by YY 0623-2008, prepare the standard solutions (7.3.1.3) and draw a calibration curve.

7.3.1.2 Fluorine standard stock solution: 100 µg/mL

The fluorine concentration of the test sample solution shall be within the concentration range of the standard solutions. If it exceeds the maximum standard solution concentration, the test sample solution shall be diluted.

7.3.2 Test method

Test the fluorine content according to 2.4.4.1 (Method 1) and 2.5 in YY 0623- 2008.

7.3.3 Result determination

The result determination shall meet the following requirements:

a) Take two samples for each product and test separately according to the above method. The two results shall comply with the provisions of 5.2.

b) If one of the two results does comply with the provisions of 5.2, take three new samples and test again. If the three results all comply with the provisions of 5.2, the item meets the requirements of this Standard, otherwise it does not meet the requirements of this Standard.

7.4.3.3 Plotting a calibration curve

Plot a calibration curve according to the following steps:

a) PIPETTE 5.0 mL of the standard solution (7.4.3.2) of each concentration into plastic containers (7.4.2.7).

b) ADD 5.0 mL of TISAB solution to each container, ADD the magnetic rotor (7.4.2.3), and STIR thoroughly.

c) INSERT the fluorine electrode and the reference electrode (7.4.2.6) into the liquid in the plastic container containing the first standard solution.

d) When the potential is stable, READ the potential value in millivolts, to the nearest 0.1 mV.

e) MEASURE the potential at least twice until the difference between the two readings is less than 0.2 mV.

f) Follow the steps c) ~ e) to measure other standard solutions.

g) PLOT a calibration curve between the millivolt potential and the logarithm of the fluoride ion concentration of the standard solutions (7.4.3.2).

NOTE: The calibration curve shall be a straight line, and the slope of the curve shall not be less than 55 mV per gradient (-log10[F]), and the determination coefficient (r2) shall be greater than 0.98.

7.4.3.4 Sample preparation

Prepare sample solutions according to the following steps:

a) OPEN the lid of a chloroform-resistant bottle (7.4.2.1) with a lid, such as a weighing bottle, and PLACE it on the balance and back to zero.

b) WEIGH about 0.05 g ~ 0.15 g of resin type product to the bottom of the container (7.4.2.1).

c) WEIGH and RECORD the mass of the resin type product, to the nearest 0.0001 g.

d) If the resin type product contains silicon fluoride, ADD 1 mol/L of KOH (7.4.1.5) to the container containing the resin type product, and MIX for 5 minutes. If the fluoride varnish does not contain silicon fluoride, skip this step.

b) The fluorine concentration (mmol/g) in the product is equal to [Fdil] multiplied by 100 and then divided by the mass of the resin product.

NOTE: When calculating the fluorine concentration in 7.4.3.3b), since the standard solution and the sample solution get the same dilution, the volume factor of 50 % dilution due to the addition of TISAB is usually ignored. If the calibration curve calculation formula uses the actual fluorine concentration (contains 50 % of TISAB dilution factor), then when calculating the fluoride ion concentration in the sample solution, this factor is applied to the calculation in 7.4.4b), where 100 is replaced by 200.

c) [mgF/g] = [F]mmol/g × 19000.

d) [mgNaF/g] = [F]mmol/g × 41990.

e) Mass fraction of fluorine = [mgF/g]/10000.

f) Mass fraction of sodium fluoride = [mgNaF/g]/10000.

7.5 Total content of heavy metals

It shall be carried out according to the heavy metal inspection method of the "Pharmacopoeia of the People's Republic of China" (2015 edition) Volume IV 0821, and shall comply with the provisions of 5.4.

7.6 Arsenic content

It shall be carried out according to the arsenic salt inspection method or equivalent method of the "Pharmacopoeia of the People's Republic of China" (2015 edition) Volume IV 0822, and shall comply with the provisions of 5.5.

7.7 Microbial content

It shall be carried out according to the provisions of microbial limit inspection of non-sterile products of the "Pharmacopoeia of the People's Republic of China" (2015 edition) Volume IV 1105 ~ 1107, and shall comply with the provisions of 5.6.

8.1 Outer packaging

The product shall include at least the following information:

a) product name, model, specification;