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GBZT317.1-2018: Determination of cadmium in blood -- Part 1: Graphite furnace atomic absorption spectrometry method
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Determination of cadmium in blood -- Part 1: Graphite furnace atomic absorption spectrometry method
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GBZ/T 317.1-2018
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Basic data | Standard ID | GBZ/T 317.1-2018 (GBZ/T317.1-2018) | | Description (Translated English) | Determination of cadmium in blood -- Part 1: Graphite furnace atomic absorption spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 7,745 | | Date of Issue | 2018-08-16 | | Date of Implementation | 2019-01-01 | | Older Standard (superseded by this standard) | WS/T 34-1996 | | Regulation (derived from) | State-Health-Communication (2018) No.14 | | Issuing agency(ies) | National Health and Family Planning Commission | GBZ/T 317.1-2018: Determination of cadmium in blood -- Part 1: Graphite furnace atomic absorption spectrometry method
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Determination of cadmium in blood - Part 1. Graphite furnace atomic absorption spectrometry method
ICS 13.100
C 52
Replace WS/T 34-1996
Determination of cadmium in blood
Part 1. Graphite furnace atomic absorption spectrometry
Determination of cadmium in blood-
Part 1. Graphite furnace atomic absorption spectrometry method
Published on.2018-08-16
2019-01-01 implementation
National Health and Wellness Committee of the People's Republic of China
National Occupational Health Standards
Foreword
This standard is formulated in accordance with the Law of the People's Republic
GBZ /T 317 "Determination of Cadmium in Blood" is divided into two parts.
-- Part 1. Graphite furnace atomic absorption spectrometry.
-- Part 2. Inductively coupled plasma mass spectrometry.
This part is the first part of GBZ /T 317.
This part is drafted in accordance with the rules given in GB/T 1.1-2009.
This section replaces WS/T 34-1996 "Method for the determination of cadmium in blood by graphite furnace atomic absorption spectrometry".
The main changes compared to WS/T 34-1996 are as follows.
-- Improved standard formulation and sample handling methods.
This section is mainly drafted by. China Center for Disease Control and Prevention, Occupational Health and Poison Control Institute, Guangdong Provincial Occupational Disease Prevention and Treatment Institute, Jiangsu
Provincial Center for Disease Control and Prevention, Shandong Institute of Occupational Health and Occupational Diseases.
The main drafters of this section. Pan Yajuan, Ding Chunguang, Zhang Aihua, Dong Ming, Zhu Alco, Liu Dezhen, Xu Guang.
The previous versions of the standards replaced by this section.
--WS/T 34-1996.
Determination of cadmium in blood - Part 1. Graphite furnace atomic absorption spectrometry
1 Scope
This part of GBZ /T 317 specifies graphite furnace atomic absorption spectrometry for the determination of cadmium in blood.
This section applies to the determination of cadmium and its compounds in the blood of occupational contacts.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this document.
For undated references, the latest edition (including all amendments) applies to this document.
GBZ /T 295 General rules for occupational health biological monitoring
3 Principle
Blood samples (hereinafter referred to as blood samples) were extracted with a nitric acid solution and determined by graphite furnace atomic absorption spectrometry at a wavelength of 228.8 nm.
The concentration of cadmium.
4 instruments
4.1 Blood collection supplies. disposable blood collection needle, sterile cotton swab, lithium heparin (sodium) vacuum blood collection tube, etc.
4.2 Volumetric flask. 5mL.
4.3 stoppered polyethylene centrifuge tube. 1.5mL.
4.4 Vortex mixer.
4.5 Centrifuge. The speed is greater than 10000r/min.
4.6 Micropipette. The range is 20μL～200μL and 100μL～1000μL.
4.7 Atomic Absorption Spectrometer. with graphite furnace, cadmium hollow cathode lamp and background correction device. Refer to Table 1 for instrument operation reference conditions.
Table 1 Instrument operation reference conditions
step
temperature
Heating time
Residence time
Carrier gas flow
mL/min
Drying 110 5 10 250
Drying 130 10 20 250
Ashing 500 20 30 250
Atomic 1800 0 3 0
Clear 2300 1 5 250
Note. The above conditions are provided for the convenience of standard users. If the conditions are changed, the same effect should be achieved.
5 reagent
5.1 Deionized water, medical alcohol.
5.2 Nitric acid, excellent grade pure, ρ20=1.42g/mL.
5.3 Nitric acid solution, 0.2% (volume fraction).
5.4 Nitric acid solution, 1% (volume fraction).
5.5 Nitric acid solution, 5% (volume fraction).
5.6 Heparin anticoagulated bovine blood, stored at -20 ° C, shake to room temperature when used. Heparin anticoagulated sheep blood can also be used. Background cadmium content should be
Less than 0.2 μg/L.
5.7 Standard solution. Nationally approved cadmium monolith standard solution.
6 Sample collection, transportation and storage
6.1 Environmental conditions. The blood collection site should be clean and tidy, and there is no source of cadmium pollution.
6.2 Personnel requirements. After rigorous training and familiarity with the blood collection process, wear powder-free latex gloves.
6.3 Sample collection. Sample collection is performed according to GBZ /T 295. Clean blood with 0.2% nitric acid solution, deionized water and medical alcohol
For the skin of the site, the blood sample should be collected more than 2 mL, and shake immediately to prevent clot formation in the blood. Collect duplicate samples if necessary,
One copy as a backup sample.
6.4 Sample blank. randomly take 2 parts of the blood collection container with the same batch number as the sample collection, and use the same batch of blood collection needle to extract 2.0 mL of deionized water.
In the blood collection tube, it is used as a sample blank.
6.5 Sample transportation. Store the collected samples and sample blanks in a clean container for refrigerated transport.
6.6 Sample storage. The sample can be stored for half a year at -20 °C.
7 Analysis steps
7.1 Preparation of blood cadmium working curve series
The cadmium monolith standard solution was diluted to 1.0 μg/mL cadmium standard application solution with 1% nitric acid solution, and then the concentration was 0.0 μg/L, 25.0.
Gg/L, 50.0 μg/L, 100.0 μg/L,.200.0 μg/L, 300.0 μg/L cadmium standard solution series (medium is 1% nitric acid solution).
Take another 6 mL volumetric flasks, numbered 1 to 6. Add 0.20 mL of cadmium standard solution series at a concentration of 0.0 μg/L to 300.0 μg/L, respectively.
Then use bovine blood to make up to the scale, and prepare the concentration to be 0.0 μg/L, 1.0 μg/L, 2.0 μg/L, 4.0 μg/L, 8.0 μg/L, 12.0 μg/L
Blood cadmium working curve solution series. See Table 2 for details.
Table 2 blood cadmium working curve solution series preparation
Number 1 2 3 4 5 6
Cadmium standard solution series concentration/(μg/L) 0.0 25.0 50.0 100.0.200.0 300.0
Cadmium standard solution series volume/mL 0.20 0.20 0.20 0.20 0.20 0.20
Bovine blood volume/mL 4.80 4.80 4.80 4.80 4.80 4.80
Blood cadmium working curve solution concentration/(μg/L) 0.0 1.0 2.0 4.0 8.0 12.0
7.2 Pretreatment of blood cadmium working curve solution series, sample and sample blank
7.2.1 Blood cadmium working curve solution series treatment. 0.15 mL blood cadmium working curve solution series was respectively centrifuged in 1.5 mL stoppered polyethylene
In the tube, add 0.60 mL of 5% nitric acid solution to each tube, cover immediately, shake vigorously, and then shake on a vortex mixer for 5 min.
Centrifuge at 10,000 r/min for 5 min and take the supernatant for measurement.
7.2.2 Sample and sample blank processing. The sample dilution factor should be consistent with the dilution factor of the working curve. Freeze blood sample or sample blank
Remove and return to laboratory temperature. Shake well and mix well. Take 0.15 mL and place in a 1.5 mL stoppered polyethylene centrifuge tube.
The same steps as above. At the same time, the reagent blank was taken. 0.75 mL of 1% nitric acid solution was taken in a 1.5 mL stoppered polyethylene centrifuge tube, and the sample was treated.
7.3 Determination of blood cadmium working curve solution series, sample and sample blank
7.3.1 Determination of blood cadmium working curve solution series. Adjust the atomic absorption spectrometer to the best measurement state, and take 15 μL of supernatant to inject.
Each work series was measured, and each concentration was measured three times. After subtracting the absorbance value of No. 1 from the absorbance value of No. 2 to No. 6, the corresponding cadmium concentration
Degree (μg/L) plots the working curve or calculates the regression equation.
7.3.2 Determination of sample and sample blanks. Determine the sample and sample blanks by measuring the operating conditions of the blood cadmium working curve series.
After subtracting the reagent blank absorbance value from the luminosity value, the concentration of cadmium (μg/L) was calculated from the working curve or the regression equation.
7.4 Quality control of the inspection process
7.4.1 Quality control of the inspection process in accordance with GBZ /T 295. The blank measurement result should be less than the detection limit. When the test result is greater than the checkout
The time limit indicates that the sample is contaminated during collection, transportation and storage, and the batch sample should be discarded.
7.4.2 Before the blood sample is tested, two levels of blood cadmium quality control samples shall be measured simultaneously, and the quality control sample shall be processed and sampled.
Processing should be carried out in the same batch. After measuring the blood cadmium working curve solution series and drawing the working curve, first determine the quality control sample, such as quality control
The measurement result of the sample falls within a given range, and the sample can be measured. The quality control sample should be repeatedly determined after every 10 samples were measured. when
When the measurement result exceeds the given range, the first 10 samples should be re-measured.
8 calculation
Calculate the concentration of cadmium in the blood sample according to formula (1).
C = C0 (1)
In the formula.
C - concentration of cadmium in blood in micrograms per liter (μg/L);
C0 - Concentration of cadmium in blood samples obtained from the working curve or regression equation in micrograms per liter (μg/L).
9 Description
9.1 The detection limit of this method is 0.24 μg/L, the lower limit of quantification is 0.70 μg/L; the measurement range is 0.70 μg/L to 12.0 μg/L. relatively
The standard deviation ranges from 2.1% to 5.2% (n=6).
9.2 The injection volume of this method can be determined according to the specific conditions of the instrument, generally choose 10 μL ~ 20 μL.
9.3 In this method, the matrix has an influence on the measurement. The sample should be treated in the same way as the working curve series solution. If the cadmium concentration in the sample is super
After the measurement range, the blood cadmium working curve range can be increased to 24.0 μg/L, and the standard series and samples are treated by the 10-fold dilution method.
The measurement was carried out by taking 0.10 mL of blood and adding 0.90 mL of a 5% nitric acid solution.
9.4 Disposable articles such as vacuum blood collection tubes, stoppered polyethylene centrifuge tubes and micro-pump tips should also be tested by background sampling.
For use, the sampling amount of each batch number shall not be less than 10. The volumetric flask and other supplies should be soaked in the nitric acid solution of 1..1 overnight, followed by tap water,
The background is detected by deionized water cleaning and the method of adding 1% nitric acid solution as the liquid to be tested, and the detection result should be less than the detection limit.
9.5 EDTA anticoagulation tubes cannot be used for blood collection tubes.
9.6 The quality control of the testing process shall be carried out in accordance with the requirements of GBZ /T 295.
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