YY/T 0823-2020 English PDF (YYT0823-2020)

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YY/T 0823-2020: Fluoride compounds used for dental carious prevention
YY/T 0823-2020
Fluoride compounds used for dental carious prevention
ICS 11.060.10
C33
People's Republic of China Pharmaceutical Industry Standard
Replace YY/T 0823-2011
Dental fluoride anti-caries material
2020-02-26 released
2021-03-01 implementation
Issued by the State Drug Administration
Preface
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces YY/T 0823-2011 "Dental Fluoride Anti-caries Materials", compared with YY/T 0823-2011, the main technical content
The changes are as follows.
---Added terms and definitions;
---The technical requirements for total fluorine content have been increased;
---The content of the detection method of total fluorine content has been added;
---Applicable product types with soluble fluorine content have been increased;
---The content of 6.2.2.2 is deleted;
---Change the microbial limit technical requirements and testing methods (in accordance with the.2015 edition of the Pharmacopoeia of the People's Republic of China);
---Edited changes to other content;
---The article number of the full text has been adjusted.
This standard uses the redrafting method to refer to ISO 17730.2014 "Dental Fluorine Paint", which is consistent with ISO 17730.2014
The degree is not equivalent.
Please note that certain contents of this document may involve patents. The issuing agency of this document shall not be responsible for identifying these patents.
This standard was proposed by the State Drug Administration.
This standard is under the jurisdiction of the National Standardization Technical Committee for Dental Materials and Devices (SAC/TC99).
This standard was drafted. Peking University School of Stomatology Dental Medical Device Inspection Center, Beijing Tianyi Hengkang Medical Devices Co., Ltd.
The main drafters of this standard. Zhang Dianyun, Lin Hong, Zhang Wei, Wang Yongfu.
The previous versions of the standard replaced by this standard are as follows.
---YY/T 0823-2011.
introduction
This standard does not contain the qualitative and quantitative requirements for possible biological hazards, but it is recommended to refer to the
YY/T 0268 "Biological Evaluation of Dental Medical Devices Unit 1 Evaluation and Testing".
This standard does not include the performance requirements and testing methods of other fluorine-containing materials (such as resins, pit and fissure sealants) other than fluoride anti-caries materials.
These requirements and methods should follow the corresponding product standards, but you can refer to this standard when determining the fluorine content.
Dental fluoride anti-caries material
1 Scope
This standard specifies the performance requirements and inspection methods of dental fluoride anti-caries materials.
This standard applies to dental materials that use fluoride as an active ingredient to prevent dental caries.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 6682-2008 Analytical laboratory water specifications and test methods
YY 0623-2008 Method for determination of soluble fluoride in dental materials
ISO 11609.2010 Dentistry toothpaste equipment test method and packaging
ISO 17730.2014 Dental Fluorine Paint
Pharmacopoeia of the People's Republic of China (2015 edition)
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Solublefluoride
Water-soluble fluoride anti-caries material can dissolve fluorine in water.
3.2
Fluoridevarnish
Coatable liquid oral material containing fluoride, topical application on the outer surface of teeth and fillings, mainly used to prevent dental caries
Bad or reduce dentine hypersensitivity.
Note. Refer to ISO 17730.2014(E).
3.3
Total fluorine
The mass fraction of fluorine in resin products of fluoride anti-caries material.
Note. Refer to ISO 17730.2014(E).
4 categories
According to the dosage form, it is divided into water-soluble type and resin type.
---Water-soluble products (such as gels, liquids, foams, pastes), directly apply to the tooth surface or contact with the tooth tray with the help of the tooth surface, and rinse with water after use
Wash it up.
---Resin-based products (such as fluorine paint), applied on the surface of the tooth, and formed a film on the tooth surface after use.
5 requirements
5.1 pH
According to 7.2 test, the pH of the sample should be in the range of 3 to 10.5, unless the manufacturer specifies and instructions otherwise.
5.2 Leachable fluorine content (applicable to water-soluble products)
According to 7.3 test, the deviation value of the soluble fluorine content of the sample should not exceed ± 10% of the value specified by the manufacturer. Unless otherwise specified by the manufacturer.
5.3 Total fluorine content (applicable to resin-based products)
According to the method specified in 7.4 or other equivalent methods, the deviation of the total fluorine content from the package nominal value should not exceed the package nominal value
±20%.
5.4 Total content of heavy metals (as Pb)
According to the method of 7.5, the total heavy metal content of the sample (calculated as Pb) should be less than 20mg/kg.
5.5 Arsenic content
According to the method of 7.6, the arsenic content of the sample should be less than 5mg/kg.
5.6 Microbial limit (applicable to water-soluble products)
5.6.1 The total number of aerobic bacteria. not more than 102CFU/g or not more than 102CFU/mL.
5.6.2 The total number of molds and yeasts. not more than 101CFU/g or not more than 101CFU/mL.
5.6.3 Pseudomonas aeruginosa. not detectable.
5.6.4 Staphylococcus aureus. not detectable.
5.6.5 Escherichia coli. Not detectable.
Note. 101CFU. indicates that the maximum acceptable number of bacteria is 20.
102CFU. indicates that the maximum acceptable bacterial count is.200.
6 sampling
The tested samples should be taken from the same batch number of retail packaging or multiple packaging materials, and the quantity can meet the required test and necessary repetition
test.
7 Test method
7.1 General
All tests should be carried out under the conditions of temperature (23±2)℃ and humidity (50±5)%, unless otherwise specified. If it is a refrigerated material
The materials should be placed in the test environment at least 4h in advance.
The water used in the test and deionized water should be in accordance with GB/T 6682-2008 Grade II water.
7.2 pH
7.2.1 Appliances
7.2.1.1 Acidity meter and pH electrode, accuracy. pH 0.02.
7.2.1.2 Plastic sheet, polyethylene or polytetrafluoroethylene sheet with a size of 60mm×20mm, the thickness is not less than 0.30mm.
7.2.2 Test procedure
The test steps are as follows.
a) Measure the pH of the sample with a pH meter and a pH electrode (7.2.1.1), rinse the electrode thoroughly after each measurement, until the displayed number is connected
Near the blank solution, proceed to the next sample test.
b) Water-soluble samples such as gels, liquids, pastes. immerse the sample in the test tip of the pH electrode, and wait for the pH meter to display at least stable value
1min, read the value.
c) For samples with a large consistency, it is advisable to take one sample and add three parts of water (weight ratio) in accordance with the method in 5.2.1 of ISO 11609.2010.
Mix well, and read the value when the pH meter shows a stable value for 1 min.
d) Foam type. Open the container with the sample, pour the liquid part at the bottom of the container into a 20mL beaker, so that the liquid is immersed in the pH electrode.
At the extreme test end, read the value when the pH meter shows a stable value for 1 min.
e) Resin type. Take a clean plastic sheet (7.2.1.2), and draw a horizontal line 20mm from one end of the plastic sheet, from the other end to the horizontal line,
Coat a layer of samples on both sides of the plastic sheet at a time, and treat or cure in accordance with the method specified in the instructions. If not specified in the manual
For the post-coating treatment method, after the coating is completed, hang it at (37±2)℃ for 5min. Hang all the surface with the sample
Hang and immerse it in a plastic beaker filled with 25mL of water and magnetic stirring, and stir at 300r/min for 5min. The pH electrode
The test tip is immersed in the above solution, and the value is read when the pH meter shows a stable value for 1 min.
7.2.3 Results judgment
The results are determined as follows.
a) Two samples are taken for each product, and the results of both times meet the requirements of 5.1, which meets the requirements of the standard.
b) If one of the two results does not meet the requirements of 5.1, take three new samples and test again. The three results all meet the requirements of 5.1.
set. The project meets the requirements of this standard, otherwise it does not meet the requirements of this standard.
7.3 Leachable fluorine content
7.3.1 Calibration working curve
7.3.1.1 Total ionic strength adjustment buffer (TISABⅡ).
7.3.1.2 Fluorine standard stock solution. 100μg/mL.
7.3.1.3 Standard solution. 0.1μg/mL, 0.5μg/mL, 1μg/mL, 5μg/mL, 10μg/mL, 20μg/mL, 50μg/mL.
7.3.1.4 According to the equipment and test methods required by YY 0623-2008, prepare a standard solution (7.3.1.3) and draw a calibration curve.
The fluorine concentration of the tested sample solution should be within the concentration range of the standard solution. If it exceeds the maximum standard solution concentration, the tested sample solution should be
dilution.
7.3.2 Detection method
Detect the fluorine content according to 2.4.4.1 (Method 1) and 2.5 in YY 0623-2008.
7.3.3 Result judgment
The result is determined to meet the following requirements.
a) Take two samples for each sample and test separately according to the above method. The two results should meet the requirements of 5.2.
b) If one of the two results does not meet the requirements of 5.2, take three more samples and test again, and the three results should meet 5.2
The project meets the requirements of this standard, otherwise it does not meet the requirements of this standard.
7.4 Total fluorine content
7.4.1 Reagents and solutions
7.4.1.1 Total ionic strength adjustment buffer (TISAB).
Note. TISABⅡ. Sodium chloride 5.8% (mass fraction), acetic acid 5.7% (mass fraction), CDTA 0.4% (mass fraction), use 5mol/L of hydrogen and oxygen
Adjust the pH to 5.0~5.5 with sodium hydroxide. For example, TISABⅡ (OrionReserch).
7.4.1.2 50% diluted TISAB solution, dilute TISAB with deionized water at a volume ratio of 1.1.
7.4.1.3 Sodium fluoride standard solution stock solution, 0.10mol/L standard sodium fluoride solution.
7.4.1.4 Trichloromethane, analytically pure.
7.4.1.5 Potassium hydroxide, 1mol/L.
7.4.2 Apparatus
7.4.2.1 Trichloromethane-resistant container with lid, the volume is 25mL or more than 25mL.
7.4.2.2 Balance with an accuracy of 0.0001g.
7.4.2.3 Magnetic rotor.
7.4.2.4 Magnetic stirrer.
7.4.2.5 Pipette, can pipette 1mL solution, accurate to 0.01mL.
7.4.2.6 Fluoride ion electrode (F-ISE), equipped with a reference electrode, or a composite electrode of F-ISE/reference electrode.
7.4.2.7 Plastic containers, plastic bottles, beakers or small containers, with a volume of at least 25mL.
7.4.2.8 pH/mV potentiometer (acidity meter), sensitivity ±0.1mV.
7.4.3 Test procedure
7.4.3.1 Environmental conditions
Test at (23±2)℃.
7.4.3.2 Preparation of standard solution
Continuously dilute the stock solution of sodium fluoride standard solution (7.4.1.3) to prepare sodium fluoride concentration of 10-2mol/L, 10-3mol/L, 10-4mol/L,
10-5mol/L standard solution.
7.4.3.3 Drawing calibration curve
Follow the steps below to draw a calibration curve.
a) Pipette 5.0 mL of the standard solution (7.4.3.2) of each concentration into a plastic container (7.4.2.7).
b) Add 5.0mLTISAB solution to their respective containers, 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 0.1mV.
e) Measure the potential at least twice until the difference between the two readings is less than 0.2mV.
f) Follow the steps c)~e) to measure other standard solutions.
g) Draw a calibration curve between the millivolt potential and the logarithm of the fluoride ion concentration of the standard solution (7.4.3.2).
Note. The calibration curve should be a straight line, and the slope of the curve should not be less than 55mV per gradient (-log10[F]), and the coefficient of determination (r2) should be greater than 0.98.
7.4.3.4 Sample preparation
Follow the steps below to prepare the sample solution.
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 to zero.
b) Weigh about 0.05g~0.15g resin type product to the bottom of the container (7.4.2.1).
c) Weigh and record the mass of the resin-based product to the nearest 0.0001g.
d) If the resin-based product contains silicon fluoride, add 1mol/L KOH (7.4.1.5) to the container containing the resin-based product,
And mix for 5 minutes, if the fluorine paint does not contain fluoride silicon, skip this step.
e) Add (4±0.5) mL of chloroform (7.4.1.4) to the container and stir.
f) Add (10.0±0.1) mLTISAB buffer to the chloroform sample.
g) Cover the lid and shake the mixture fully, dissolve the resin-based product in chloroform, and dissolve all the fluorine in TISAB, loosen
The cap releases the pressure in the bottle for a short time and then recap it.
h) Join the magnetic rotor (7.4.2.3).
i) Stir at room temperature for at least 1.5h.
Note. In some cases, TISAB/chloroform/resin products are not sufficiently dissolved under magnetic stirring. If necessary, put the spinner in the sample bottle.
Or shake the vial for better mixing.
j) Turn off the magnetic...