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Determination of cadmium in blood -- Part 2: Inductively coupled plasma mass spectrometry method
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GBZ/T 317.2-2018
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Basic data | Standard ID | GBZ/T 317.2-2018 (GBZ/T317.2-2018) | | Description (Translated English) | Determination of cadmium in blood -- Part 2: Inductively coupled plasma mass spectrometry method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 6,639 | | Date of Issue | 2018-08-16 | | Date of Implementation | 2019-01-01 | | Regulation (derived from) | State-Health-Communication (2018) No.14 | | Issuing agency(ies) | National Health and Family Planning Commission |
GBZ/T 317.2-2018: Determination of cadmium in blood -- Part 2: Inductively coupled plasma mass spectrometry method ---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of cadmium in blood - Part 2. Inductively coupled plasma mass spectrometry method
ICS 13.100
C 52
Determination of cadmium in blood
Part 2. Inductively coupled plasma mass spectrometry
Determination of cadmium in blood-
Part 2. Inductively coupled plasma mass 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 second part of GBZ /T 317.
This part is drafted in accordance with the rules given in GB/T 1.1-2009.
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 standard. Pan Yajuan, Ding Chunguang, Zhang Aihua, Dong Ming, Zhu Alco, Liu Dezhen, Xu Guang.
Determination of cadmium in blood - Part 2. Inductively coupled plasma mass spectrometry
1 Scope
This part of GBZ /T 317 specifies inductively coupled plasma mass 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 directly diluted with 0.5% nitric acid/0.01% Triton X-100 mixture to give 铑 (Rh, 10.0 μg/L)
As an internal standard, the concentration of cadmium in the diluent was measured by inductively coupled plasma mass spectrometry.
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. 5 mL.
4.3 Polyethylene centrifuge tube. 15 mL.
4.4 Vortex mixer.
4.5 Micropipette. The range is from 100 μL to 1000 μL.
4.6 Inductively Coupled Plasma Mass Spectrometer. equipped with an autosampler.
Instrument operation reference conditions.
-- cooling gas flow rate. 12.5 L/min;
-- Auxiliary gas flow rate. 0.70 L/min;
- atomization gas flow rate. 0.88 L/min;
- peristaltic pump speed. 30 r/min;
-- Nebulizer temperature. 3 °C.
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.
5.2 Nitric acid, excellent grade pure, ρ20=1.42 g/mL; nitric acid solution, 0.2% (volume fraction).
5.3 0.5% nitric acid/0.01% Triton X-100 mixed solution.
5.4 Heparin anticoagulated bovine blood, stored at -20 °C, shake to room temperature when used. Heparin anticoagulated sheep blood can also be used. The background cadmium content should be lower than
0.2 μg/L.
5.5 Standard solution. Adopt nationally recognized standard solution of cadmium and strontium.
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. 0.2% nitric acid solution, deionized water, and clean skin of the blood collection site, the blood sample should be collected more than 2 mL, and
Shake immediately to prevent clot formation in the blood. Collect duplicate samples as necessary and 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 water into the blood collection tube.
Medium, 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 standard series
The cadmium monolith standard solution was diluted to 1.0 μg/mL cadmium standard application solution with 0.5% nitric acid solution, and then the concentration was 0.0 μg/L.
0.1 μg/L, 1.0 μg/L, 10.0 μg/L, 100.0 μg/L cadmium standard solution series (medium is 0.5% nitric acid solution).
7.2 Pretreatment of blood cadmium samples and sample blanks
Remove the frozen blood sample or sample blank and return to laboratory temperature. Shake well and mix well, take 0.50 mL, and place in 15 mL polyethylene
In the centrifuge tube, add 4.50 mL of 0.5% nitric acid/0.01% Triton X-100 mixed solution and shake for testing. At the same time as a reagent blank, the same sample
deal with.
7.3 Determination of blood cadmium standard solution series, samples and sample blanks
7.3.1 Determination of blood cadmium standard solution series. ICP-MS is adjusted to the best measurement state, each standard solution is determined, and each concentration is repeatedly measured.
Set 2 times. The working curve is calculated or the regression equation is calculated for the corresponding cadmium concentration (μg/L) by the count value (excluding the reagent blank).
7.3.2 Determination of sample and sample blanks. The sample and sample blanks are determined by the operating conditions of the measurement work series, and the count value is subtracted from the reagents.
After white, the concentration of cadmium (μg/L) was calculated from a standard curve or a regression equation.
7.4 Quality control of the inspection process
7.4.1 The blank measurement result should be less than the detection limit. When the test result is greater than the detection limit, it indicates that the sample is in the process of collection, transportation and storage.
If contaminated, batch samples should be discarded.
7.4.2 Before the blood sample test, two levels of blood cadmium quality control samples shall be measured simultaneously, and the quality control sample processing and sample processing shall be performed.
Should be carried out in the same batch. After measuring the blood cadmium standard solution series and drawing a standard curve, first measure the quality control sample, such as the quality control sample.
The determination results fall within a given range and sample determination can be performed. The quality control sample should be repeatedly determined after every 10 samples were measured. When the measurement result
When the given range is exceeded, the first 10 samples should be re-measured.
8 calculation
Calculate the concentration of cadmium in the blood sample according to formula (1).
C = F × C0 (1)
In the formula.
C - the concentration of cadmium in the blood, in micrograms per liter (μg/L);
F - sample dilution factor (10 in this method);
C0 - The concentration of cadmium in a blood sample calculated from a standard curve or a regression equation in micrograms per liter (μg/L).
9 Description
9.1 The detection limit of this method is 0.08 μg/L, the lower limit of quantification is 0.30 μg/L; the measurement range is 0.30 μg/L to 1000.00 μg/L (in
Blood sample 10 times diluted). The relative standard deviation ranged from 2.60% to 8.70% (n=6).
9.2 Single-use items such as vacuum blood collection tubes, polyethylene centrifuge tubes and micro-pump tips should also be used after sampling.
The sampling amount of each batch number shall not be less than 10. Volumetric flasks and other supplies need to be soaked overnight in 1..1 nitric acid solution, followed by tap water, deionized
The water is cleaned, and the background test is carried out by adding 0.5% nitric acid solution as the liquid to be tested, and the test result should be less than the detection limit.
9.3 The EDTA anticoagulation tube cannot be used for blood collection tubes.
9.4 The quality control of the testing process shall be carried out in accordance with the requirements of GBZ /T 295.
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