GB/T 14233.1-2022 PDF in English
GB/T 14233.1-2022 (GB/T14233.1-2022, GBT 14233.1-2022, GBT14233.1-2022)
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Test methods for infusion, transfusion, injection equipments for medical use -- Part 1: Chemical analysis methods
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| GB/T 14233.1-2008 | English | 135 |
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Test methods for infusion, transfusion, injection equipment for medical use -- Part 1: Chemical analysis methods
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Infusion, transfusion, injection equipment for medical use--Part 1: Chemical analysis methods
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Infusion, transfusion, injection equipment for medical use--Part 1: Chemical analysis methods
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GB/T 14233.1-2022: PDF in English (GBT 14233.1-2022) GB/T 14233.1-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 11.040.20
CCS C 31
Replacing GB/T 14233.1-2008
Test Methods for Infusion, Transfusion, Injection Equipment
for Medical Use - Part 1: Chemical Analysis Methods
ISSUED ON: OCTOBER 12, 2022
IMPLEMENTED ON: NOVEMBER 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword ... 3
Introduction ... 5
1 Scope ... 6
2 Normative References ... 6
3 Terms and Definitions ... 6
4 General Rules ... 6
5 Analysis Methods of Extractable Matters of Test Solution ... 9
6 Analysis Method of Total Content of Heavy Metals in the Materials... 19
7 Content Analysis Methods of Some Heavy Metal Elements in the Materials ... 20
8 Residue on Ignition ... 22
9 Determination of Ethylene Oxide Residue - Gas Chromatography ... 23
Bibliography ... 27
Test Methods for Infusion, Transfusion, Injection Equipment
for Medical Use - Part 1: Chemical Analysis Methods
1 Scope
This document specifies the chemical analysis methods for the infusion, transfusion and
injection equipment for medical use.
This document is applicable to the chemical analysis of the infusion, transfusion, injection and
supporting equipment for medical use and made of medical polymer materials. The chemical
analysis of other medical polymer products can also take this document as a reference.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in this text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 601 Chemical Reagent - Preparations of Standard Volumetric Solutions
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
Pharmacopoeia of the People’s Republic of China (Version 2020) Four Volumes
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 General Rules
4.1 Overview
4.1.1 All analyses in this document are carried out in two parallel test groups; the results shall
be within the allowable relative deviation limit; the arithmetic mean shall be taken as the
determination result. If one is qualified and the other is disqualified, the average calculation
shall not be performed and the determination shall be re-performed.
4.1.2 Unless it is otherwise specified, all reagents used in this document are analytically pure.
4.1.3 Unless it is otherwise specified, the test water in this document shall comply with the
requirements of Grade-2 water in GB/T 6682.
4.1.4 The term “room temperature” used in this document refers to 10 C ~ 30 C.
4.1.5 The term “accurate weighing” used in this document refers to weighing accurate to 0.1
mg.
4.1.6 The term “accurate measuring” used in this document refers to measuring with a transfer
pipette that complies with the accuracy requirements specified in the corresponding national
standards.
4.1.7 Constant weight by gravimetric method means that the weight difference of the test
sample after two consecutive ignitions or dryings shall not exceed 0.3 mg.
4.1.8 Unless it is otherwise specified, the glass containers used in this document are all
borosilicate glass containers.
4.1.9 Most of the analysis methods provided in this document are non-specific analysis methods,
and these methods can be used for the preliminary assessment of chemical hazards of medical
devices. However, if there is a situation that does not comply with the preliminary expectations
in a specific test, it does not suggest that the actual risk is unacceptable, and specific analysis
methods need to be adopted to identify and evaluate the safety.
4.2 Preparation of Test Solution
4.2.1 The preparation of the test solution shall simulate the conditions (such as: the application
area, time and temperature of the product, etc.) that the product goes through during the using
process as much as possible. The simulated extraction time shall not be less than the normal
use time of the product. When the product has been used for a long time (more than 24 h),
consideration should be given to prepare the test solution under accelerated test conditions, but
the feasibility and rationality need to be verified.
4.2.2 The methods used for the preparation of the test solution should try to extract all the tested
surfaces of the sample.
4.2.3 It is recommended to select the test solution preparation method in Table 1, and:
---If the sample preparation conditions in the brackets are used, it shall be indicated in the
product standard;
---The selection of temperature should take into account the highest temperature that the
product may be subject to in clinical use. For polymers, the temperature shall be
selected below the glass transition temperature.
solution and dilute to the required concentration.
Silver nitrate test solution (17.5 g/L): weigh-take 1.75 g of silver nitrate, dissolve it in water,
dilute to 100 mL and store it in a brown bottle.
Nitric acid solution: take 105 mL of nitric acid and use water to dilute to 1,000 mL.
5.3.3 Test procedures
Accurately measure-take 10 mL of the test solution, add it to a 50 mL Nessler colorimetric tube;
add 10 mL of dilute nitric acid (if the solution is not clear, filter it and place the filtrate in a 50
mL Nessler colorimetric tube), add water to make it about 40 mL. Thus, the test solution is
obtained.
Accurately measure-take 10 mL of the chlorine standard solution to another 50 mL Nessler
colorimetric tube; add 10 mL of dilute nitric acid; add water to make it about 40 mL; shake it
well. Thus, the standard control solution is obtained.
In the above-mentioned two test tubes, respectively add 1.0 mL of silver nitrate test solution,
use water to dilute to 50 mL; place it in a dark place for 5 min; place it on a black background
and observe from above the colorimetric tube. Compare the turbidity of the test solution with
the standard control solution.
If the test solution is colored, unless it is otherwise specified, take two portions of the test
solution and respectively place them in a 50 mL Nessler colorimetric tube. Add 1.0 mL of silver
nitrate test solution to one portion, shake it well and let it stand for 10 min. If it becomes turbid,
repeatedly filter it, until the filtrate is completely clear. Then, add the specified amount of
chlorine standard solution and an appropriate amount of water to make it 50 mL; shake it well
and place it in the dark for 5 min; use it as the control solution. Add 1.0 mL of silver nitrate test
solution to another portion and an appropriate amount of water to make it 50 mL. Shake it well
and place it in the dark for 5 min. In accordance with the above-mentioned method, compare it
with the control solution. Thus, the solution is obtained.
5.4 pH
5.4.1 Method 1
Take the test solution and the blank control solution. In accordance with the 0631 pH value
determination method of Pharmacopoeia of the People’s Republic of China (Version 2020) Four
Volumes, respectively determine the pH value and take the difference between them as the test
result.
5.4.2 Method 2
5.4.2.1 Solution preparation
Sodium hydroxide standard titration solution [c (NaOH) = 0.1 mol/L]: in accordance with the
stipulations of GB/T 601, prepare and titrate it.
Sodium hydroxide standard titration solution [c (NaOH) = 0.01 mol/L]: before use, take the
sodium hydroxide standard titration solution [c (NaOH) = 0.1 mol/L] and add water to dilute
10 times.
Hydrochloric acid standard titration solution [c (HCl) = 0.1 mol/L]: in accordance with the
stipulations of GB/T 601, prepare and titrate it.
Hydrochloric acid standard titration solution [c (HCl) = 0.01 mol/L]: before use, take the
hydrochloric acid standard titration solution [c (HCl) = 0.1 mol/L] and add water to dilute 10
times.
Tashiro indicator: dissolve 0.2 g of methyl red and 0.1 g of methylene blue in 100 mL of
methanol (with a volume fraction of 95%).
5.4.2.2 Test procedures
Accurately measure-take 20 mL of the test solution and place it in a 100 mL ground-mouth
bottle; add 0.1 mL of Tashiro indicator. If the color of the solution turns purple, then, use the
sodium hydroxide standard titration solution [c (NaOH) = 0.01 mol/L] to titrate it; if it turns
green, use the hydrochloric acid standard titration solution [c (HCl) = 0.01 mol/L] to titrate it,
until it turns gray. Take the volume (in mL) of the consumed sodium hydroxide standard
titration solution [c (NaOH) = 0.01 mol/L] or hydrochloric acid standard titration solution [c
(HCl) = 0.01 mol/L] as the test result.
5.4.3 Method 3
5.4.3.1 Solution preparation
Sodium hydroxide standard titration solution [c (NaOH) = 0.1 mol/L]: same as 5.4.2.1.
Sodium hydroxide standard titration solution [c (NaOH) = 0.01 mol/L]: same as 5.4.2.1.
Hydrochloric acid standard titration solution [c (HCl) = 0.1 mol/L]: same as 5.4.2.1.
Hydrochloric acid standard titration solution [c (HCl) = 0.01 mol/L]: same as 5.4.2.1.
Phenolphthalein indicating solution (10 g/L): weigh-take 1 g of phenolphthalein, dissolve it in
ethanol (with a volume fraction of 95%) and dilute to 100 mL.
Methyl red indicating solution (1 g/L): weigh-take 0.1 g of methyl red, dissolve it in ethanol
(with a volume fraction of 95%) and dilute to 100 mL.
5.4.3.2 Test procedures
Add 2 drops of the phenolphthalein indicating solution to 10 mL of test solution, and the
solution shall not turn red. Add 0.4 mL of the sodium hydroxide standard titration solution [c
(NaOH) = 0.01 mol/L], and the solution shall turn red. Add 0.8 mL of the hydrochloric acid
standard titration solution [c (HCl) = 0.01 mol/L], and the red color shall disappear. Add 5 drops
store it in the refrigerator. Before use, take 5 mL of the mixed solution [composed of 15 mL of
sodium hydroxide (1 mol/L), 5 mL of water and 20 mL of glycerin], add 1 mL of the above-
mentioned thioacetamide solution; place it on a water bath to heat for 20 s, cool it down and
immediately use it.
Lead standard stock solution (0.1 mg/mL): weigh-take 0.160 g of lead nitrate, use 10 mL of
nitric acid solution (1 + 9) to dissolve it, then, transfer it into a 1,000 mL volumetric flask and
use water to dilute to the scale.
Lead standard solution: before use, accurately measure-take the lead standard stock solution
and dilute it to the required concentration.
5.6.1.3 Test procedures
Accurately measure-take 25 mL of the test solution in a 25 mL Nessler colorimetric tube; take
another 25 mL Nessler colorimetric tube and add 25 mL of the lead standard solution.
Respectively add 2 mL of acetate buffer solution (pH 3.5) to the above-mentioned two
colorimetric tubes, then, respectively add 2 mL of thioacetamide test solution, let it stand for 2
min. Place it on a white background and observe from above; compare the color shades.
If the test solution develops color, a small amount of dilute caramel solution or other non-
interfering colored solutions can be added to the standard control solution, so as to make it
consistent with the color of the test solution. Then, respectively add 2 mL of thioacetamide test
solution to the test solution and the standard control solution; shake it well and let it stand for
2 min. Place it on a white background and observe from above; compare the color shades.
Alternatively, take 10 mL of the test solution, then, the amount of lead standard solution added
is 10 mL.
5.6.2 Method 2
5.6.2.1 Principle
In an alkaline solution, heavy metals, such as: lead, chromium, copper and zinc, can react with
sodium sulfide to generate insoluble colored sulfides. Take lead as a representative to prepare
a standard solution for colorimetric comparison and determine the total content of the heavy
metals.
5.6.2.2 Solution preparation
Sodium hydroxide test solution (43 g/L): take 4.3 g of sodium hydroxide and add water to
dissolve it to 100 mL. Thus, the solution is obtained.
Sodium sulfide test solution (100 g/L): before use, weigh 1 g of sodium sulfide and add water
to dissolve it to 10 mL. Thus, the solution is obtained.
Lead standard stock solution (0.1 mg/mL): same as 5.6.1.2.
Lead standard solution: same as 5.6.1.2.
5.6.2.3 Test procedures
Accurately measure-take 25 mL of the test solution in a 25 mL Nessler colorimetric tube; take
another 25 mL Nessler colorimetric tube and add 25 mL of the lead standard solution.
Respectively add 5 mL of the sodium hydroxide test solution to the above-mentioned two
colorimetric tubes, then, respectively add 5 drops of the sodium sulfide test solution and shake
it well. Place it on a white background and observe from above; compare the color shades.
5.7 UV Absorbance
Take the test solution, if necessary, use a 0.45 m microporous filter membrane to filter it.
Within 5 h, use a 1 cm cuvette with the blank control solution as a reference. Within the
specified wavelength range, determine the absorbance.
5.8 Ammonium
5.8.1 Principle
Ammonium ions can react with Nessler reagent in alkaline solution to generate a yellow
substance. Through colorimetric comparison with the standard control solution, determine its
ammonium content.
5.8.2 Solution preparation
Sodium hydroxide solution (40 g/L): weigh-take 4.0 g of sodium hydroxide, use water to
dissolve and dilute it to 100 mL.
Nessler reagent (alkaline potassium mercuric iodide test solution): take 10 g of potassium iodide,
add 10 mL of water to dissolve it, then, slowly add a saturated aqueous solution of mercuric
dichloride, stir as it is added, until the generated red precipitate is no longer dissolved. Add 30
g of potassium hydroxide and dissolve it, then, add 1 mL or above of a saturated aqueous
solution of mercuric dichloride, and use an appropriate amount of water to dilute it to 200 mL;
let it stand and precipitate. Thus, the solution is obtained. During use, pour off the supernatant.
Inspection: take 2 mL of this solution, add it to 50 mL of water containing 0.05 mg of ammonia,
and it shall immediately appear yellowish brown.
Ammonium standard stock solution (0.1 mg/mL): weigh-take 0.297 g of ammonium chloride
dried to a constant mass at 105 C ~ 110 C; use water to dissolve and dilute it to 1,000 mL.
Ammonium standard solution: before use, accurately measure-take the ammonium standard
stock solution and dilute to the required concentration.
5.8.3 Test procedures
Accurately measure-take 10 mL of the test solution in a 25 mL Nessler colorimetric tube; take
another 25 mL Nessler colorimetric tube and add 10 mL of the ammonium standard solution.
5.9.3 Atomic fluorescence spectrometry
5.9.3.1 Instrument
Atomic fluorescence spectrophotometer. During use, operate it in accordance with the
instruction manual.
5.9.3.2 Analysis method (standard curve method)
Within the concentration range recommended by the atomic fluorescence spectrophotometer,
at least 5 standard solutions (excluding the zero point) containing the elements to be determined
and with increasing concentrations in sequence shall be prepared. The concentration range of
the standard solutions should consider the concentration of the element to be determined. Then,
take the solvent used to prepare the standard solutions as a blank and successively determine
the fluorescence intensity of each standard solution; draw a standard curve relative to the
concentration.
Determine the test solution and the blank control solution. In accordance with the absorbance,
find out the corresponding concentration on the standard curve; calculate the content of the
element.
6 Analysis Method of Total Content of Heavy Metals in the
Materials
6.1 Principle
In a weakly acidic solution, heavy metals, such as: lead, cadmium, copper and zinc, can react
with thioacetamide to generate insoluble colored sulfides. By taking lead standard solution as
the standard for colorimetric comparison, their total content can be determined.
6.2 Preparation of Reagents and Solutions
Comply with 5.6.1.2.
6.3 Preparation of Test Solution
Take an appropriate amount of sample and cut into pieces of 5 mm 5 mm; put it into a
porcelain crucible; slowly blaze it, until it is completely charred, and let it cool. Then, add 0.5
mL ~ 1 mL of sulfuric acid to moisten it. At a low temperature, heat it, until the sulfuric acid
vapor disappears. Then, add 0.5 mL of nitric acid and evaporate it to dryness; after the nitrogen
oxide vapor is completely removed, let it cool. Then, at 500 C ~ 600 C, burn it to make it ash;
after it cools down. Add 2 mL of hydrochloric acid, place it on a water bath and evaporate it to
dryness, then add 15 mL of water. Add one drop of phenolphthalein test solution, then, dropwise
add the ammonia test solution, until the above-mentioned solution turns reddish. Add 2 mL of
acetate buffer solution (pH 3.5) and slightly heat to dissolve it (if there is any residue, it should
be filtered with filter paper), then, transfer the solution to a 25 mL Nessler colorimetric tube;
add water to make 25 mL of test solution.
Place another porcelain crucible added with 0.5 mL ~ 1 mL of sulfuric acid, 0.5 mL of nitric
acid and 2 mL of hydrochloric acid on a water bath to evaporate it to dryness. Add 2 mL of
acetate buffer solution (pH 3.5) and 15 mL of water, slightly heat to dissolve it, then, transfer
the solution to a 25 mL Nessler colorimetric tube. Add a certain amount of lead standard
solution, then, use water to dilute it to 25 mL; take it as the standard control solution.
6.4 Test Procedures
Respectively add 2 mL of thioacetamide test solution to the test solution and the standard
control solution; shake it well and let it stand for 2 min. On a white background, observe it from
above and compare the color shades.
If the test solution develops color, a small amount of dilute caramel solution or other non-
interfering colored solutions can be added to the standard control solution to make it consistent
with the color of the sample solution.
7 Content Analysis Methods of Some Heavy Metal Elements
in the Materials
7.1 Atomic Absorption Spectrophotometry
7.1.1 Sample digestion
7.1.1.1 Wet digestion: take 1 g ~ 2 g of sample, accurately weigh it and cut it into pieces of
about 5 mm 5 mm; place it in a 100 mL conical flask, add 30 mL of nitric acid and 1.25 mL
of sulfuric acid, shake it well and place it overnight; heat it on a hot plate for digestion. If there
are still undecomposed substances or the color becomes darker when the digestion solution
reaches about 10 mL, remove it and let it come down. Add 5 mL ~ 10 mL of nitric acid, then,
digest it to about 10 mL for observation. Repeat this two or three times, and pay attention to
avoid charring. Cool it down, add 25 mL of water, then evaporate it, until white fumes of
sulfuric acid are emitted. Cool it down, then, use water to transfer the content to a 50 mL
volumetric flask; add water to obtain 50 mL of test solution. Use the same method to prepare
the blank control solution.
7.1.1.2 Dry-ashing: take 1 g ~ 2 g of sample, accurately weigh it and place it in a crucible. Add
10 mL of magnesium nitrate solution with a mass concentration of 150 g/L and mix it well. At
low heat, evaporate it to dryness. Carefully cover 1 g of magnesium oxide on the dry residue,
char it, until there is no black smoke, then, at 550 C, ash it for 4 h. Take it out and let it cool;
carefully add 10 mL of hydrochloric acid (1 + 1) to neutralize the magnesium oxide and dissolve
the ash (if there is any residue, it should be filtered with filter paper). Transfer it to a 50 mL
volumetric flask, and add water to make 50 mL of test solution. Use the same method to prepare
the blank control solution.
9 Determination of Ethylene Oxide Residue - Gas
Chromatography
9.1 Instrument
Gas chromatograph. During use, operate it in accordance with the instruction manual.
9.2 Analysis Method
Any gas chromatography can be used as long as the analysis is proven to be reliable. “Analytical
reliability” means that when determining a device with a specified residual amount of ethylene
oxide (EO), the selected analysis method has sufficient accuracy, precision, selectivity, linearity
and sensitivity, and suitable for the device to be analyzed.
For different products, necessary methodological evaluation is required to determine the
reliability of the selected method.
Other validated analysis methods may also be adopted, for example, mass spectrometry.
9.3 Sample Extraction Methods
9.3.1 General rule
There are three basic sample extraction methods for the determination of ethylene oxide residue
on medical devices sterilized with ethylene oxide: simulated use extraction method, stringent
extraction method and extreme extraction method.
The simulated use extraction method refers to the method that makes the extraction simulate
the use of the product as much as possible. This simulation process allows the measured residual
ethylene oxide to correspond to the actual ethylene oxide intake of the patient using the device.
The stringent extraction method is an extraction that is expected to result in the release of greater
or a larger amount of chemical constituents than under clinical use conditions.
The extreme extraction method means that the amount of ethylene oxide determined in the
second extraction is less than 10% of the value determined in the first extraction, or the
cumulative residual amount determined by extraction has no obvious increase.
The extract should be prepared after sampling, otherwise, the test sample shall be sealed in a
metal container sealed with polytetrafluoroethylene for preservation.
When citing the method of this document, if no extraction method is specified, then, it shall be
carried out in accordance with the extreme extraction method or the stringent extraction method.
9.3.2 Simulated use extraction method
9.4.3 Draw a standard curve
Use the stock solution to prepare standard solutions with at least 5 series of concentrations
ranging from 1 g/mL ~ 20 g/mL. Accurately measure-take 5 mL and place it in a 20 mL
extraction vessel, seal it; at a constant temperature (60 C 1 C), balance it for 40 min.
Use a sample injector to successively and quickly take the upper part of gas from the balanced
standard sample, inject it into the sample injection chamber and record the peak height (or area)
of ethylene oxide. Draw a standard curve (X: mass concentration of ethylene oxide, g/mL; Y:
peak height or area).
9.4.4 Measurement of test sample
Use the sample injector to quickly take the upper part of gas from the balanced specimen
extraction vessel, inject it into the sample injection chamber and record the peak height (or area)
of ethylene oxide.
In accordance with the standard curve, calculate the corresponding concentration of the sample.
If the result of the measured sample is beyond the range of the standard curve, the concentration
of the standard solution shall be changed to re-draw the standard curve.
9.4.5 Recommended chromatographic conditions
Chromatographic column: the stationary phase is generally 6% cyanopropyl benzene and 94%
dimethyl siloxane.
Injection port temperature: 200 C.
Column flow rate: 1.5 mL/min.
Detector: FID.
Split ratio: 20 : 1.
Column oven temperature: maintain at 50 C for 8 min.
Detector temperature: 250 C.
Other validated chromatographic conditions may also be adopted.
9.5 Result Calculation
The residual amount of ethylene oxide is expressed by the absolute content or relative content.
9.5.1 In accordance with Formula (5), calculate the absolute content of ethylene oxide per unit
of product:
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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