YY/T 1555.2-2018 English PDF (YYT1555.2-2018)

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YY/T 1555.2-2018: Particular requirements for the silicone gel filled breast implant - Performance requirement of silicone gel filler - Part 2: Limits requirement for extractable substances
YY/T 1555.2-2018
Particular requirements for the silicone gel filled breast implant. Performance requirement of silicone gel filler-Part 2.Limits requirement for extractable substances
ICS 11.040.30
C30
People's Republic of China Pharmaceutical Industry Standards
Specific requirements for silicone gel-filled breast implants
Silicon gel filling performance requirements
Part 2.Limit requirements for extractable substances
2018-12-20 released
2020-01-01 Implementation
Issued by the National Medical Products Administration
Specific requirements for silicone gel-filled breast implants
Silicon gel filling performance requirements
Part 2.Limit requirements for extractable substances
1 Scope
This part of YY/T 1555 specifies the extraction method and detection of the extractable substances in the silicone gel filling used for artificial breast implants
Method and limit requirements.
This section applies to artificial breast implants with silicone gel as the inner filling.
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 reference documents, the latest version (including all amendments) is applicable to this standard.
YY 0334-2002 General requirements for silicone rubber surgical implants
YY/T 1457 Method for determination of oligopolysiloxanes in silicone gel-filled breast implants for passive surgical implants
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Breast implant
An implant with a shell used to increase breast volume or replace breasts, which can be filled into the shell by the manufacturer or surgeon
Charge objects.
[YY 0647-2008, definition 3.5]
3.2
Filler filer
The contents of the implant.
3.3
Silicone gel
A type of low modulus gel material composed of low-degree cross-linked polysiloxane.
3.4
Extractingsubstances
Use a suitable solvent to extract the substances mentioned from the silicone gel under the specified extraction conditions.
4 Limit requirements
4.1 pH
The absolute value of the difference between the pH of the sample water extract and the blank control solution should not be greater than 1.5.
4.2 Reducing substances (easy oxides)
For the addition type silicone gel, the sample water extract and the blank control solution consume potassium permanganate solution [c(KMnO4)=0.002mol/L]
The difference in volume should not exceed 3.0mL.
4.3 Peroxide
For thermally vulcanized silicone gel, the sample extract and blank control solution consume sodium thiosulfate solution [c(Na2S2O3)=0.01mol/L]
The difference in volume should not exceed 0.2mL.
4.4 UV absorbance
The absorption value of the sample water extract in the wavelength range of 220nm~340nm does not exceed 0.1.
4.5 Heavy metals
The total heavy metal content of the sample water extract (calculated as Pb2) should not exceed 1 mg/L.
4.6 Evaporation residue
The evaporation residue of 100mL sample water extract should not exceed 2mg.
4.7 Residual amount of oligosiloxane substances
The residual amount of octamethylcyclotetrasiloxane (D4) should not exceed 50mg/kg.
The residual amount of decamethylcyclopentasiloxane (D5) should not exceed 50mg/kg.
5 Detection method
5.1 pH
Prepare the extract according to Appendix A, A.1, and perform the test according to the method in YY 0334-2002 Appendix C.
5.2 Reducing substances (easy oxides)
Prepare the extract according to A.1, and perform the test according to the method in YY 0334-2002 Appendix E.
5.3 Peroxide
Prepare the extract according to A.2, and test it according to the method in Appendix D of YY 0334-2002.
5.4 UV absorbance
Prepare the extract according to A.1, and perform the test according to the method in Appendix F of YY 0334-2002.
5.5 Heavy metals
Prepare the extract according to A.1, and perform the test according to the method in Appendix G of YY 0334-2002.
5.6 Evaporation residue
Prepare the extract according to A.1, take 100 mL of the extract, add it to an evaporating dish that has been dried to a constant weight at 105°C, evaporate to dryness and heat at 105°C
Dry to constant weight in a constant temperature box, and measure the blank control solution by the same method.
5.7 Residual amount of oligosiloxane substances
Prepare the extract according to A.3, test it according to the method of YY/T 1457, or test it according to the method of Appendix B.
Appendix A
(Normative appendix)
Preparation method of extract
A.1 Preparation method of water extract
Take out an appropriate amount of silicone gel from the breast implant, weigh it with a balance, add purified water at the ratio of 1g sample to 20mL purified water, and
Leave it at (37±2)℃ for (72±2)h in a water bath, separate the liquid part and filter it with filter paper to obtain the water extract. With the same batch of purified water
Method to prepare blank control solution.
A.2 Preparation method of dichloromethane extract
Take out an appropriate amount of silicone gel from the breast implant, weigh it with a balance, and add dichloromethane at the ratio of 1g sample to 20mL dichloromethane
Alkane, seal, and let it stand for (72±2)h in a water bath at (37±2)℃ to obtain the dichloromethane extract. Prepare empty space with the same batch of dichloromethane and the same method
White control solution.
A.3 Preparation method of acetone extract
Take out an appropriate amount of silicone gel from the breast implant, weigh it with a balance, and add 5 mL of acetone to 1g sample at a ratio of (37±2)°C
Ultrasonic leaching for 30min, cooling to room temperature and filtering with a 0.45μm organic filter membrane to obtain the test solution. Prepare blank control solution in the same way.
Note. Organic solvents are volatile, so the volatilization of solvents needs to be controlled during the test operation.
Appendix B
(Normative appendix)
Determination of residual oligosiloxane substances. gas chromatography (GC method)
B.1 Principle
Gas chromatography was used to analyze the small molecules in the extract. When the vaporized sample is brought into the chromatographic column by the mobile phase for operation,
The two phases are repeatedly distributed multiple times. Because the distribution coefficients of the components in the mobile phase and the stationary phase are different, each component is in the chromatographic column.
The operating speeds of the two are different, and they are separated from each other after a certain length of the column. Leave the chromatographic column and enter the detector in order.
The component information of the product is converted into an electrical signal, and the size of the electrical signal is proportional to the amount or concentration of the measured component, so as to realize the measurement of the measured component.
Detection.
B.2 Apparatus
B.2.1 Gas chromatograph with hydrogen flame ionization detector.
B.2.2 Electronic balance (precision 0.1mg).
B.2.3 Ultrasonic cleaner.
B.3 Reagents
B.3.1 Acetone, requires analytical grade and above.
B.3.2 Octamethylcyclotetrasiloxane (D4) requires analytical grade and above.
B.3.3 Decamethylcyclopentasiloxane (D5), requires analytical grade and above.
B.4 Test method
B.4.1 Standard solution preparation
Take about 0.05g each of D4, D5 and other oligosiloxane substances, accurately weigh them, and dilute to 50 mL with acetone, and then use the solution
Dilute acetone in sequence to form at least 5 concentration gradients of D4 and D5 oligosiloxane substances with a concentration of 1μg/mL~50μg/mL
Mix the standard solution.
B.4.2 Gas phase determination
Chromatographic conditions.
Chromatographic column. 5% phenyl-95% polydimethylsiloxane as a fixed liquid capillary column (30m×0.25mm×0.25μm);
Column temperature. 60°C (hold for 3min), raise to 300°C at 10°C/min (hold for 10min);
Inlet temperature. 280℃;
Detector temperature. 300℃;
Carrier gas. helium or nitrogen (purity above 99.99%), flow rate 1.0mL/min;
Injection volume. 1μL.
Take the blank solution, standard solution, and sample solution (see A.3 for the preparation method) for the gas chromatograph test, and take a standard solution with an intermediate concentration.
The quasi-solution was injected 5 times continuously, and the relative standard deviation RSD of the peak area of oligosiloxane substances was calculated.
B.5 Result analysis
B.5.1 Use the external standard method to analyze the test results, establish a standard working curve and regression equation, and calculate the
Residual amount of polysiloxane-like substances. The measurement result is expressed as the ratio of the mass (μg) of oligosiloxane substances to the mass (g) of the test.
The unit is μg/g, that is, mg/kg.
X=c×V/m (B.1)
Where.
X --- The residual amount of oligosiloxane substances, in micrograms per gram (μg/g, that is, mg/kg);
c ---The concentration value of oligosiloxane substances in the sample test solution read on the standard curve, in micrograms per milliliter (μg/mL);
V --- The volume of the added extraction solvent acetone, in milliliters (mL);
m ---The mass of the sample, in grams (g).
B.5.2 If the concentration value read on the standard curve is less than the minimum concentration value of the standard solution, the result is expressed by formula (B.2).
X \u003ccmin×V/m (B.2)
Where.
X --- The residual amount of oligosiloxane substances, in micrograms per gram (μg/g, that is, mg/kg);
cmin --- the minimum concentration value of the standard solution, in micrograms per milliliter (μg/mL);
V --- The volume of the added extraction solvent acetone, in milliliters (mL);
m ---The mass of the sample, in grams (g).
B.5.3 Methodological requirements.
a) The linear correlation coefficient R of the standard curve equation of oligosiloxane substances should not be less than 0.995;
b) The resolution of oligosiloxane substances on the chromatogram should not be less than 1.5;
c) Repeatability of the method. The relative standard deviation RSD of the peak area of oligosiloxane substances should not be greater than 10%.
Note. If other low molecular weight substances other than D4 and D5 are detected in the sample, they should also be analyzed.