BJS201706-2017 PDF English
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Determination of chlorate and perchlorate in food
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Similar standards BJS 201706 BJS201706-2017: Determination of chlorate and perchlorate in food---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/BJS201706-2017
Attachment 2
BJS
Determination of chlorate and perchlorate in food
Table of Contents
1 Scope... 3
2 Principle... 3
3 Reagents and materials... 3
4 Apparatus... 5
5 Specimen preparation and storage... 6
6 Determination procedure... 7
7 Result calculation... 11
8 Sensitivity, accuracy and precision of the detection method... 11
Appendix A Schematic diagram of purification method... 13
Appendix B Characteristic ion chromatograms of chlorate and perchlorate... 14
Determination of chlorate and perchlorate in food
1 Scope
This method specifies the liquid chromatography-tandem mass spectrometry
for the determination of chlorate and perchlorate content in food.
This method is applicable to the determination of chlorate and perchlorate in
packaged drinking water, liquid milk, rice, carrots, cantaloupe, pork, fish, tea,
infant formula milk powder (excluding infant formula milk powder for special
medical purposes).
2 Principle
After the specimen is extracted and centrifuged, use a solid-phase extraction
column to purify the supernatant; USE liquid chromatography-tandem mass
spectrometry to determine; USE the internal standard method to quantify.
3 Reagents and materials
3.1 Reagents
3.1.1 Acetonitrile (CH3CN). Chromatographically pure.
3.1.2 Methanol (CH3OH). Chromatographically pure.
3.1.3 Formic acid (HCOOH). Chromatographically pure.
3.1.4 Ammonium formate (HCOONH4). LC-MS grade.
3.1.5 Ultrapure water (H2O). The resistivity is 18.2 MΩ·cm.
3.2 Reagent preparation
3.2.1 Aqueous solution containing 0.1% formic acid. MEASURE 1.0 mL of
formic acid (3.1.3) to a 1000 mL volumetric flask; USE ultrapure water (3.1.5)
to dilute to the mark and mix well.
3.3 Standards
3.3.1 Sodium chlorate standard. USE certified standards or high-purity
reagents; the purity is >99%. The Chinese name, English name, CAS registry
number, molecular formula, and relative molecular weight are given in Table 1.
3.4 Isotope internal standards
3.4.1 Chlorate isotope internal standard. Chlorate-18O3 (200 μg/mL, in terms of
chlorate-18O3 ion, provided by Beijing Bestown, EURL-SRMLotNo.024), stored
at 4 °C.
3.5.5 Mixed standard working solutions. Accurately measure 0 μL, 10 μL, 25 μL,
50 μL, 75 μL, 100 μL, 250 μL, 500 μL, 750 μL, 1000 μL of mixed standard
intermediate solution (3.5.3) respectively AND 100 μL of mixed isotope internal
standard solution (3.5.4).
4 Apparatus
4.1 Liquid chromatograph-tandem mass spectrometer, equipped with
electrospray ion source (ESI source).
4.2 Vortex oscillator.
4.3 Tissue masher.
4.4 Homogenizer.
4.8 Centrifuge tube with stopper. 50 mL.
4.9 PRiMEHLB solid-phase extraction column. 3cc, 150 mm; or those with
equivalent performance.
Note. Before use, 4.8 and 4.9 consumables shall be tested for background.
5 Specimen preparation and storage
5.1 Packaged drinking water
MIX well and use directly.
5.3 Pork and fish.
TAKE an appropriate amount of representative edible specimen; CUT it into
small pieces; USE a tissue masher to mash them; DIVIDE equally them into
two, as the specimen and the reserved specimen. PUT them into clean
containers, respectively; SEAL and mark them; and store them at -18 °C in the
dark.
5.4 Carrot and cantaloupe.
TAKE an appropriate amount of representative specimens; REMOVE the peel
and seeds, and cut into small pieces.
5.5 Infant formula milk powder.
MIX well; TAKE an appropriate amount of representative specimen; DIVIDE
equally into two, as the specimen and the reserved specimen. PUT them into
clean containers, respectively; SEAL and mark them; and store them at room
temperature in the dark.
5.6 Rice and tea.
TAKE an appropriate amount of representative specimens; after being crushed
by a pulverizer, pass through a 40-mesh sieve. DIVIDE equally into two, as the
specimen and the reserved specimen. PUT them into clean containers,
respectively; SEAL and mark them; and store them at room temperature in the
dark.
6 Determination procedure
6.1 Extraction
6.1.1 Packaged drinking water.
Accurately pipette 1.0 mL of specimen; ADD 10.0 μL of mixed isotope internal
standard solution (3.5.4); vortex-oscillate for 10 s. After filtration through a 0.22
μm regenerated cellulose filter membrane, take the subsequent filtrate for
determination by liquid chromatograph-tandem mass spectrometer.
6.1.5 Liquid milk.
Accurately weigh 5 g (accurate to 0.001 g) of the specimen into a 50 mL
centrifuge tube with stopper (4.8). ADD 150 μL of mixed isotope internal
standard solution (3.5.4); ADD 1.0 mL of 0.1% formic acid aqueous solution
(3.2.1), 9.0 mL of methanol (3.1.2); vortex-oscillate for 5 min. Centrifuge at
10000 r/min at room temperature for 10 min; TAKE the supernatant for
purification.
6.3 Chromatographic determination
6.3.1 Liquid chromatography-tandem mass spectrometry detection
6.3.1.2 Reference mass spectrometric conditions
6.3.4 Quantitative determination
Collision energy (eV) Cone voltage (V) Daughter ion (m/z) Parent ion (m/z) Compound
6.4 Blank test
Except that no specimen is added, the operation is performed in the same
manner as the specimen.
7 Result calculation
The result is calculated according to formula (1).
8 Sensitivity, accuracy and precision of the detection method
8.1 Sensitivity
When the specimen size is 1.0 mL, the detection limit of chlorate in packaged
drinking water is 0.6 μg/L; the limit of quantification is 2.0 μg/L. The detection
limit of perchlorate is 0.4 μg/L; the limit of quantification is 1.0 μg/L.
8.2 Accuracy
Within the fortified concentration range of 5~800 μg/kg, the recovery rate of this
method is 80%~110%.
8.3 Precision
The absolute difference between two independent determination results,
obtained under repeatability conditions, must not exceed 20% of the arithmetic
mean.
BJS201706-2017
Attachment 2
BJS
Determination of chlorate and perchlorate in food
Table of Contents
1 Scope... 3
2 Principle... 3
3 Reagents and materials... 3
4 Apparatus... 5
5 Specimen preparation and storage... 6
6 Determination procedure... 7
7 Result calculation... 11
8 Sensitivity, accuracy and precision of the detection method... 11
Appendix A Schematic diagram of purification method... 13
Appendix B Characteristic ion chromatograms of chlorate and perchlorate... 14
Determination of chlorate and perchlorate in food
1 Scope
This method specifies the liquid chromatography-tandem mass spectrometry
for the determination of chlorate and perchlorate content in food.
This method is applicable to the determination of chlorate and perchlorate in
packaged drinking water, liquid milk, rice, carrots, cantaloupe, pork, fish, tea,
infant formula milk powder (excluding infant formula milk powder for special
medical purposes).
2 Principle
After the specimen is extracted and centrifuged, use a solid-phase extraction
column to purify the supernatant; USE liquid chromatography-tandem mass
spectrometry to determine; USE the internal standard method to quantify.
3 Reagents and materials
3.1 Reagents
3.1.1 Acetonitrile (CH3CN). Chromatographically pure.
3.1.2 Methanol (CH3OH). Chromatographically pure.
3.1.3 Formic acid (HCOOH). Chromatographically pure.
3.1.4 Ammonium formate (HCOONH4). LC-MS grade.
3.1.5 Ultrapure water (H2O). The resistivity is 18.2 MΩ·cm.
3.2 Reagent preparation
3.2.1 Aqueous solution containing 0.1% formic acid. MEASURE 1.0 mL of
formic acid (3.1.3) to a 1000 mL volumetric flask; USE ultrapure water (3.1.5)
to dilute to the mark and mix well.
3.3 Standards
3.3.1 Sodium chlorate standard. USE certified standards or high-purity
reagents; the purity is >99%. The Chinese name, English name, CAS registry
number, molecular formula, and relative molecular weight are given in Table 1.
3.4 Isotope internal standards
3.4.1 Chlorate isotope internal standard. Chlorate-18O3 (200 μg/mL, in terms of
chlorate-18O3 ion, provided by Beijing Bestown, EURL-SRMLotNo.024), stored
at 4 °C.
3.5.5 Mixed standard working solutions. Accurately measure 0 μL, 10 μL, 25 μL,
50 μL, 75 μL, 100 μL, 250 μL, 500 μL, 750 μL, 1000 μL of mixed standard
intermediate solution (3.5.3) respectively AND 100 μL of mixed isotope internal
standard solution (3.5.4).
4 Apparatus
4.1 Liquid chromatograph-tandem mass spectrometer, equipped with
electrospray ion source (ESI source).
4.2 Vortex oscillator.
4.3 Tissue masher.
4.4 Homogenizer.
4.8 Centrifuge tube with stopper. 50 mL.
4.9 PRiMEHLB solid-phase extraction column. 3cc, 150 mm; or those with
equivalent performance.
Note. Before use, 4.8 and 4.9 consumables shall be tested for background.
5 Specimen preparation and storage
5.1 Packaged drinking water
MIX well and use directly.
5.3 Pork and fish.
TAKE an appropriate amount of representative edible specimen; CUT it into
small pieces; USE a tissue masher to mash them; DIVIDE equally them into
two, as the specimen and the reserved specimen. PUT them into clean
containers, respectively; SEAL and mark them; and store them at -18 °C in the
dark.
5.4 Carrot and cantaloupe.
TAKE an appropriate amount of representative specimens; REMOVE the peel
and seeds, and cut into small pieces.
5.5 Infant formula milk powder.
MIX well; TAKE an appropriate amount of representative specimen; DIVIDE
equally into two, as the specimen and the reserved specimen. PUT them into
clean containers, respectively; SEAL and mark them; and store them at room
temperature in the dark.
5.6 Rice and tea.
TAKE an appropriate amount of representative specimens; after being crushed
by a pulverizer, pass through a 40-mesh sieve. DIVIDE equally into two, as the
specimen and the reserved specimen. PUT them into clean containers,
respectively; SEAL and mark them; and store them at room temperature in the
dark.
6 Determination procedure
6.1 Extraction
6.1.1 Packaged drinking water.
Accurately pipette 1.0 mL of specimen; ADD 10.0 μL of mixed isotope internal
standard solution (3.5.4); vortex-oscillate for 10 s. After filtration through a 0.22
μm regenerated cellulose filter membrane, take the subsequent filtrate for
determination by liquid chromatograph-tandem mass spectrometer.
6.1.5 Liquid milk.
Accurately weigh 5 g (accurate to 0.001 g) of the specimen into a 50 mL
centrifuge tube with stopper (4.8). ADD 150 μL of mixed isotope internal
standard solution (3.5.4); ADD 1.0 mL of 0.1% formic acid aqueous solution
(3.2.1), 9.0 mL of methanol (3.1.2); vortex-oscillate for 5 min. Centrifuge at
10000 r/min at room temperature for 10 min; TAKE the supernatant for
purification.
6.3 Chromatographic determination
6.3.1 Liquid chromatography-tandem mass spectrometry detection
6.3.1.2 Reference mass spectrometric conditions
6.3.4 Quantitative determination
Collision energy (eV) Cone voltage (V) Daughter ion (m/z) Parent ion (m/z) Compound
6.4 Blank test
Except that no specimen is added, the operation is performed in the same
manner as the specimen.
7 Result calculation
The result is calculated according to formula (1).
8 Sensitivity, accuracy and precision of the detection method
8.1 Sensitivity
When the specimen size is 1.0 mL, the detection limit of chlorate in packaged
drinking water is 0.6 μg/L; the limit of quantification is 2.0 μg/L. The detection
limit of perchlorate is 0.4 μg/L; the limit of quantification is 1.0 μg/L.
8.2 Accuracy
Within the fortified concentration range of 5~800 μg/kg, the recovery rate of this
method is 80%~110%.
8.3 Precision
The absolute difference between two independent determination results,
obtained under repeatability conditions, must not exceed 20% of the arithmetic
mean.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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