YY 0334-2002 General requirements for silicone rubber surgical implants
Some standard content:
Pharmaceutical Industry Standard of the People's Republic of China
YY 0334
General specification for silicone surgical implants
2002-04-25 Issued
Issued by the State Food and Drug Administration
2002-10-01 Implementation
YY0334—2002
This standard is modified and adopted from the American standard BS7253P3.1990 Specification for hot-vulcanized silicone surgical implants. The controlled items are less than those of the British standard, including zinc, beryllium, diamond, copper, pin, manganese, aluminum, wedge, vanadium and knot. The maximum requirements of this standard are stricter than those of the British standard. British standard (1 mg/kg), increase the requirements of "total amount of free ions of heavy metals, easy oxidation, other requirements and so on, this standard with the appendix A ~ appendix (is the standard constant radiation record, thank you record H to the material appendix, this standard drafting unit: the National Drug War Supervision and Administration High-Economic Medical Device Quality or Supervision Inspection Center: this standard is the national drug supervision and administration exhibition won the Tang medical device quality supervision award teaching heart mouth. Wood standard who is the main drafter: Jia Zhihong, Sui Yanping, also Ke Jian. Pan Huaxian, Sun Guangyu. 1) The United States said that the library has been on the gland before. 1
YY 0334—2002
Silicone surgical implants are formed by the mixing of sulfide compounds with adhesives and various types of fillers. The physical properties, that is, the mechanical properties, of such implants (such as joint prostheses and prostheses) vary greatly. Therefore, this standard specifies the specific indicators of the physical properties of the implant. The requirements may be considered in the physical properties of most silicone implants: except for implants with or without silicone rubber components (such as shunts, membranes, and silicone-supported fabrics), the scope of the standard is limited to silicone rubber components made of silicone rubber. The physical requirements of such implants should be specified in the relevant product standards. Once inserted, it should not be used again. Elastic rubber cavity material The processing technology is not different. Unlike metal parts, which can be processed by a series of processes such as shaping, cutting, etc., silicone parts can rarely be processed by fine processing. In some cases, the parts are processed into blocks or sheets, and the required size of the parts before implantation is small. Therefore, this standard does not specify the requirements. For silicone parts that are processed into sheets, except for the requirements for packaging and marking specified in this standard, other requirements apply. 1 Standard
General requirements for silicone rubber surgical implants
YY0334—2002
This standard specifies the chemical and biological properties of silicone rubber parts such as grease, non-stick, and packaging, but does not specify the physical properties of the parts.
These parts are used for surgical shaping and repair. Surgical parts made of silicone and other materials are not included in this standard.
2 Normative references
The clauses in the following documents are considered as the standard clauses through the use of this standard. For the referenced documents with the specified date, all the subsequent amendments (excluding errors) or revisions are not applicable to this standard. However, the parties to the agreement based on this standard shall study whether the latest versions of these documents can be used. For the referenced documents without the specified date, the latest version shall apply to this standard. B691 Chemical reagents Preparation of sieve solutions for quantitative analysis (narrow quantitative separation) GHT1117: Biological verification methods for materials with certain biological properties GB/718A6.1 Biological evaluation of therapeutic agents Part 1 Evaluation and testing YY\C313 Packaging, marking, transportation and transportation of medical polymer products The terms used in this standard are defined in the Pharmacopoeia of the People's Republic of China, 2003 Edition.
Heat-vulcanization, leat-curing Silicone rubber is transformed into elastic material (silicone strand) by heating 3.2
Silicone rubber elastomer
Silicone rubber is converted into elastic material by curing or secondary curing: that is, the material with rubber properties obtained by curing or secondary curing. 3.3
Silicone rubber is a material made by combining silicone with suitable materials and crosslinking agents. This material is crosslinked. 3.4
Polysiloxane slltcenepalyllozane
Mainly composed of silicone atoms linked to each other. The chain contains organic groups. 3.5
Secondary curing is a process carried out at a certain temperature after curing to enhance the physical properties of the material and (or) remove excess decomposition products. 4 Foreign matter
The plant surface should be inspected at 1°C for 1 month without any foreign particles. 1
YY 03342002
5 Biochemical properties
5.1 General
The plant surface should be tested in the as supplied state. If there are more than two separable and unrelated types of base rubber in the product, each type of base rubber should be sampled and tested separately.
5.2 Biological evaluation
When the biological evaluation of the base rubber plant or the rubber specimens of the same fiber adding process is carried out in accordance with G/T 16886.1 and GR/T 15175, the test shows that the whole plant is non-toxic. 5.3 Material requirements
5.3.1 Loss on drying
After heating 1.0g of the extract or plant sample at 200℃ for 4h, the loss of the sample or the sample should not exceed 2.0%. 5.3.2 Micro-element content
When tested in accordance with Appendix A, the metal element content of the product should comply with the requirements of Table 1. Table 1 Content of implanted materials Metal elements Maximum limit
Trace metals
Arsenic (A9)
5.4 Requirements for dropouts
5.4.1 Residue inspection
Maximum limit/(usg/kg)
When tested according to the appendix, the residue of implants or implant samples shall comply with the provisions of Table 2. Table 2 Concurrent residue limit
Sample quantity/g
5.4.2 Hydroxypropyl alcohol
When tested according to the appendix, the difference between the implant sample and the blank value shall not be greater than 1. 5.4.3 Peroxide
Bracket (sample mass fraction)
For heat-resistant rubber products, when tested according to the appendix: the sample solution and blank solution consume sodium thiosulfate solution (centrifugal concentration) 0. 1mol/L. The volume difference should not exceed 0.2mL5.4.4 Reducing substances (i.e., chemical substances) should be less than 0.2mL for the added silicon implants. When the F test is performed, the difference between the sample and the blank in the volume of potassium manganate [r(KMnO,)c.302l should be less than 0.0m.5.4-5 Ultraviolet absorption and the absorption value in the wavelength range of 2nm.~340rD should not exceed 0.4.5.4.6 During the gold week test, the metal content should not exceed 1. E Sterile contact should be confirmed by the bacterium test process, and the Again, the description of the sterilization method. 2
Note! : The appropriate sterilization method is referenced by the reference reference, let 2: GB/T11235.2 stipulates that there is no formula for sterilization, but the formula is not directly used by the factory, YY0334-2002
Note 3: The use of Sichuan cyclohexane bacteria, the preparation of ethylene oxide, the attachment and GB/15886.7 provide the requirements for the determination of epoxy brown substances and product release. Packaging and marking
The packaging and marking of the implant shall comply with the relevant provisions of YY/T0313. Permanent surgical implants should have a unique traceable label.
YY 0334-2002
(Normative Appendix)
Test methods for trace elements
A.1 Atomic absorption spectrophotometric determination of lead, chromium and iron 4.1. Principle
The sample is dissolved in a sealed container with 1% caustic soda and 1% hydrochloric acid to prepare a test solution. The two pots of the original absorption spectrophotometer are connected vertically to determine the content of lead, chromium and iron.
4.2 Preparation of reagents and reagents
Standard solutions containing lead, chromium and iron are prepared according to the above methods: 1:1 preparation volume of the prepared solution is 1:1, diluted to the required concentration before use: 1:1 concentration of 1% caustic soda and 1:1 dilution with 1% caustic soda to obtain the required concentration.
4.1.3 Preparation of test solution
Weigh sample 2R in a flash ethylene cup and add 1l of nitric acid.Heat 1m3 of hydrochloric acid in a container for 2 hours at 1600C, cool to room temperature, add 1% ethylene, heat on an electric heater until nearly dry. Add 1% ethylene, heat again until nearly dry, add 1% ethylene by volume, heat until nearly dry, and cool. Use polyolefins to absorb, transfer the sample solution into 1% ethylene by volume solution, wash with 1% ethylene by volume solution, collect the washed solution in a bottle, and dilute to the mark with 1% ethylene by volume solution. A.1.4 Test method A.1.4.1 Determination of the content: Take the test solution prepared in A.1.3 and determine it by the pyrolysis atomic absorption method using the 1% method. Operation method: Please refer to the instrument manual. 4.1.4.2 Determination of iron content: A.1.3 Preparation of test solution: Please refer to the instrument manual. A.2 Determination of elasticity: 4.2.1 Preparation of test solution: Collect 1 ml of sodium hyaluronate powder and spread it on the bottom and around the plate. Accurately weigh the sample and place it in the middle of the plate. Stir lightly to make it contact with carbon-free steel. Add 1 ml of water to make it just moist. Evaporate the water until dry. Heat at low temperature until no more smoke appears. Cool at 350°C for about 250°C. Add 2.5 ml of sodium hyaluronate and stir to make it into a paste. A.2.2 Test method: Pour 21 mL of water into 1 CCml of test solution in several portions. Take a 7-well bottle and add 2.5 mL of the standard solution. Add 5 mL of saline and 21 mL of water. Test according to the "Test Methods" in Part II of the Pharmacopoeia of the People's Republic of China. Appendix H (Normative Appendix) Test method for residual sputum tt||The sample is extracted with natural water and deionized water at the same rate, then the benzene is removed and dried by heat. Weigh or measure the extract. B.2.1 Natural water or deionized water,
B.2.2 n-hexane [analytical grade].
B.3.1 Silicone glass pre-pressurized flow chamber
B.3.3 Water.
B.4 Test steps
B.2.1 Evaporated water extraction
YY0332002
Cut the sample into pieces less than 11) μm, weigh 24.5g~25.5g of sample with a balance, accurate to =0.-g and record the sample mass. Return the sample to the apparatus, add 100 mL of distilled water or deionized water, heat to reflux for 4 h, stop heating, cool, reflux through a sintered glass funnel, filter the solution, put it into a sealed container, transfer 100 mL of the sample to a 105% dry container, dry it and then dry it in a 105% wet box. Determine the blank control effect in the same way.
B.4.2 n-hexane extraction
If the sample is solid, cut the sample into 5 mm thick pieces, add 2.7-3.35 ml of pure water to 0.30 ml of pure water.
Add 15% n-hexane to the sample and heat to reflux for 4 h. After stopping heating, cool the sample and immediately filter it through a sintered glass funnel, filter it if necessary, and place it in an aldehyde extractor. Transfer 10 ml of the solution to be dried at 15°C until 100% evaporated water, evaporate and place in a 105°C constant temperature box for 2 hours, cool to room temperature and weigh.
B.5 Result Expression
The mass of each sample (the ratio of the original mass of the sample) is calculated according to the formula (T3.), expressed as a percentage: p=w-wxgx100
Where:
.-·The evaporated mass after adding the immersion wave and drying, in grams (g); w[-without adding the concentrated hot hemoglobin, in grams (g); m-the mass of the sample, in grams (g) converted to a cumulative value, for water, take 5; for n-hexane, take 3/2. Let, be patient with the expectation that I can, Appendix
(Normative Appendix)
Get the test method
C.1 Principle
Use a pH meter to measure the pH value of the serum and the blank control respectively, and take the difference between the two as the test result. YY53342002
C2 Potassium hydroxide (.name: L> Economic drop: Weigh potassium hydroxide, dissolve in water, dilute to 1aT. C.3 Accelerator
C.3.1 Borosilicate acid test flow device, container 1.U. .3.2 Rubber into glass tube
.4 Test steps
If it is a light solid, the sample is as small as 1) mr, report R2. Sample, extract up to 10g, record the sample mass: Place the sample in a flow device, add 5T.=.mi. Distilled water minus deionized water, heat to 51.
Stop if the system cools back to the stomach, that is, use a calciner or ton bucket to siphon, the more you get, put it in a container with added silica. Prepare the reference solution. Take 20.cm2 of the test piece and add 1.0ml of standard chloride, and use it to determine the value of the sample and the empty solution respectively. Appendix D Normative Appendix Test method for peroxide T.1 Principle The amount of ions in the sample is replaced by adding a chemical under acidic conditions. Sodium sulfate is used as an additive to dissolve the ions. D.2 Test Method D.2.1 An analytically pure form of methyl sulfoxide.
D.2.2 Prepare new sodium iodide (analytical grade>0.2p/: 25g sodium iodide in 100mL glacial acetic acid! Separate. Note: Glacial acetic acid is a strong corrosive. Proper protection should be taken when working. 2, 3 (Na) = 1mol. Flow rate: according to the standard sodium iodide in G0. 1. Calibrate: D2.4 Before the standard sodium iodide is added, add water to the standard sodium iodide and add the catalyst.
1.7.5 Prepare new indicator.
.3 Test steps
Take the sample in a small piece, weigh 4.5. At the exact time, record the sample mass, place the sample in a conical flask, add 1.m dihydrogen alkane, and disassemble the drug chamber for 16 seconds. Immediately filter through a filter, collect the product in a micro-airtight flask, and continuously add 1. (mL) sodium thiosulfate solution into the flask with no hydrogen to clear the air in the flask. Stop the flask, shake the spoon, and place it at room temperature for 30 min. Add 5. (mL) of water, mix, and add 1. (mL) of sodium thiosulfate solution dropwise, using 1. (mL) of sodium thiosulfate solution as an indicator. Record the point at which the end point is reached to an accuracy of 0.2 mT. Do not add any product above this point and perform the self-determination in the air. 5
D.4 Expression of results
The result is expressed as the difference between the test volume and the measured volume of the sodium thiosulfate solution in the test flask. If the method is repeated for more than ten minutes, the result will be expressed as follows: Normative Appendix:
Test method for reductive substances (analytical substances) E.1 Principle
Yr 334—2002
The sample solution contains a large amount of raw materials such as potassium manganate. When heated, the excess potassium carbide will oxidize potassium carbide to chlorine, and then be reduced by other acid.
E.2 Reagents
Benefits: Prepare 5=L slow-release, inject 50ml of water, dilute to 1000mL of dilute acid, add 5L of slow-release acid solution, add 1Dm.c (KMmO2).n2ml/1. High-pressure standard solution: Prepare 3.3g of manganese acid, add 1L of water, add water to 1M, and let stand for more than 2 days. Use a microporous slide to filter and measure its concentration. KMn0200.K12m./1. High-pressure standard solution: Prepare 5.02mol/1. Potassium hydrogen standard solution, dilute to 1L with water. If necessary, cool, filter, and then calibrate the precipitation indicator. Take 5 starch solution. Boil in medium and cool to standby (NS) = 0.10. Sodium thiosulfate standard solution, add 2 standard solution (NS), .5T) or sodium thiosulfate without water, boil for 1 hour at 1 cm. Cool, add water for 1 hour, filter after 1 week, and calibrate.
: (N., S) 0.nl/. Sodium thiosulfate standard solution, take .1ml/ before use, dilute with 10% sodium thiosulfate standard solution with 10% freshly boiled and cooled water.
E.3cNa25:0,)=0.1mol/L sodium thiophosphate solution is prepared by weighing accurately, adding 25ml of water to the standard soya bean paste solution, adding 20% potassium hydroxide to dilute the acid to 2% by volume, and adding 1ml of water to the dilute acid solution. Use a ruler to titrate the solution with 1ml/titration point. When the blue solution turns bright green, perform a vacuum test. E.4. Preparation of samples
Crush the sample into small pieces of 10 mm, weigh and collect more than 25 ml: Place the sample in a flow chamber, add 5 ml of moistening water or calcium ion water, heat to 5, cool after heating, and filter with a funnel. Filter the sample into a container, add the crushed pieces,
F.5 Test steps
Mixed media: Flow potassium permanganate standard solution of acid product, boil for 3.1 min, cool rapidly, add 1 iodine, plug and simmer. Titrate with sodium thiosulfate standard solution of the same concentration until yellow, add starch indicator solution, and continue to titrate with potassium permanganate standard solution until yellow. YY03342002
Determine the control strategy by the method of the company.
F.6 Calculation of the result
The content of reducing substances (products) is expressed by the amount of manganese dioxide obtained by the elimination of the sample solution. The calculation formula is: VF
Wherein:
V—the volume of the consumed higher acid (unit is liter): 1. The volume of the sample solution containing sodium thiosulfate (unit is milliliter). 1. The volume of the blank solution containing the consumed higher acid (unit is liter (mI).) The actual concentration of the diluted potassium permanganate solution (unit is mole per liter (mnl/T). C.—the concentration of potassium permanganate (c(1/SKMn) specified in the standard, unit is mn1/1). Appendix F
(Normative Appendix)
The concentration of the sample extract is in moles per liter (mn1/1). F.1 Principle
The implant or sample is calcined and the absorbance of the extract is determined by a spectrophotometer. F.2 Apparatus
F.2.1 UV spectrophotometer (range: +220 nm - 340 nm) E.2.2 Instrument with a path length of 19 mm for comparison. F.3 Test steps
If the implant or sample is solid, weigh 1.g to 2.2g of the material, grind it to -0.001g, and calcine the sample in 130 ml of hexane and reflux for 4 h.
After heating, cool it and immediately reflux it with a sterilizer. Place it in a small container with boric acid. Place the micro-liquid in a 1 cm colorimetric control and use a stopper. Scan the wavelength range of 22 nm--340 nm and record the maximum external absorption value. The result is expressed in luminance, which is the maximum value of external light absorption within the test wavelength range. Note that the accuracy of this method is ± 2. Appendix (Normative Appendix) Test method for determination of metals GT Principle In alkaline liquid: lead, chromium, copper, iron and other metals can react with sodium hydroxide to form non-uniform compounds. Standard solution is prepared with sodium hydroxide as a representative for colorimetry. The determination of heavy metals is generally agreed. G.2 Preparation and standard preparation: weigh 1598g of 110% lead hydroxide in a dryer and add 55cmL of water. Dissolve it in water until it is diluted to zero. Before use, take 1 part of the standard lead solution and sieve 1 part of each solution according to the standard lead standard (the lead content is 1n4:ml.). Chemical solution: take 13-hydroxyl hydroxide and add water to make a solution. 3. Prepare the sample: collect 10ml of sodium ion solution or weigh a sample less than 5ml in length, place the sample in a dry reflux container, add 500ml of distilled water, reflux for 5h, stop heating, cool, and then pressurize to remove the ion. If necessary, add 25ml of the sample to a Nessler colorimetric tube, add 2.5ml of standard dye solution to the sieved water until 25:10, add sodium ion solution to the test tube, fill it up to 50%, shake well, weigh it, and observe according to the color book. Compare the depth of the sample. 5 Results
Recommended
(Informative Appendix)
Test method for ethylene oxide splash retention
H.1 Conditions
Use water to remove the ethylene oxide in the sample and use headspace gas chromatography to determine the ethylene oxide content. Gas chromatograph
11.2.1 The hydrogen flame should have a sensitivity of not less than 2×:01 g benzene, carbon dioxide (S:]H.2.2 Chromatographic sample: The chromatograph used should be able to completely separate the impurities and non-oxygen in the test sample and have a certain water resistance. The chromatograph column can be selected according to the conditions recommended in Table H.1.
Table H.1 Chromatographic conditions
1 ar~-2: iri
H.2.3 Instrument - Temperature of each position:
) Vaporization chamber 230;
) Dyeing chamber 20.
3> QC5/AC:0 1. 0
CDX-2C7
Parapak ae
Model 130℃
$120℃.Screen the water to 25:10, add the oxygenated hook tester, 5% sodium chloride, shake well, check the depth of the workpiece according to the color book, and compare the depth of the amount
(i. 5 Resultswww.bzxz.net
Recommended
(Informative Appendix)
Test method for ethylene oxide splash retention
H.1 Conditions
Use water to remove the ethylene oxide in the sample and use headspace gas chromatography to determine the ethylene oxide content. Gas chromatograph
11.2.1 The hydrogen flame should have a sensitivity of not less than 2×:01 g benzene, carbon dioxide (S:]H.2.2 Chromatographic sample: The chromatograph used should be able to completely separate the impurities and non-oxygen in the test sample and have a certain water resistance. The chromatograph column can be selected according to the conditions recommended in Table H.1.
Table H.1 Chromatographic conditions
1 ar~-2: iri
H.2.3 Instrument - Temperature of each position:
) Vaporization chamber 230;
) Dyeing chamber 20.
3> QC5/AC:0 1. 0
CDX-2C7
Parapak ae
Model 130℃
$120℃.Screen the water to 25:10, add the oxygenated hook tester, 5% sodium chloride, shake well, check the color book and compare the depth of the wall
(i. 5 Results
Recommended
(Informative Appendix)
Test method for ethylene oxide splash retention
H.1 Conditions
Use water to remove the ethylene oxide in the sample and use headspace gas chromatography to determine the ethylene oxide content. Gas chromatograph
11.2.1 The hydrogen flame should have a sensitivity of not less than 2×:01 g benzene, carbon dioxide (S:]H.2.2 Chromatographic sample: The chromatograph used should be able to completely separate the impurities and non-oxygen in the test sample and have a certain water resistance. The chromatograph column can be selected according to the conditions recommended in Table H.1.
Table H.1 Chromatographic conditions
1 ar~-2: iri
H.2.3 Instrument - Temperature of each position:
) Vaporization chamber 230;
) Dyeing chamber 20.
3> QC5/AC:0 1. 0
CDX-2C7
Parapak ae
Model 130℃
$120℃
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