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HJ 1183-2021: (Water quality Determination of omethoate, methamidophos, acephate and phoxim liquid chromatography-triple quadrupole mass spectrometry)
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(Water quality Determination of omethoate, methamidophos, acephate and phoxim liquid chromatography-triple quadrupole mass spectrometry)
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HJ 1183-2021
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Basic data | Standard ID | HJ 1183-2021 (HJ1183-2021) | | Description (Translated English) | (Water quality Determination of omethoate, methamidophos, acephate and phoxim liquid chromatography-triple quadrupole mass spectrometry) | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 16,196 | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 1183-2021: (Water quality Determination of omethoate, methamidophos, acephate and phoxim liquid chromatography-triple quadrupole mass spectrometry)
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(Water quality Determination of omethoate, methamidophos, acephate and phoxim liquid chromatography-triple quadrupole mass spectrometry)
National Ecological Environment Standard of the People's Republic of China
Water quality omethoate, methamidophos, acetamide
Determination of phosphorus and phoxim
liquid chromatography-triple quadrupole mass spectrometry
Water quality-Determination of omethoate, methamidophos, acephate,
phoxim-Liquid chromatography-triple quadrupole mass spectrometry
This electronic version is the official standard text, which is reviewed and typeset by the Environmental Standards Institute of the Ministry of Ecology and Environment.
Published on 2021-06-03
2021-12-15 Implementation
Released by the Ministry of Ecology and Environment
directory
Foreword...ii
1 Scope...1
2 Normative references...1
3 Principles of the method...1
4 Interference and cancellation...1
5 Reagents and materials...1
6 Instruments and equipment...2
7 Samples...3
8 Analysis steps...3
9 Result calculation and representation...5
10 Accuracy...6
11 Quality Assurance and Quality Control...7
12 Waste Disposal...8
Appendix A (normative appendix) detection limit and lower limit of determination of the method...9
Appendix B (informative) Accuracy of the method...10
Determination of omethoate, methamidophos, acephate and phoxim in water quality
liquid chromatography-triple quadrupole mass spectrometry
Warning. Some solvents and standards used in the experiment have certain toxicity. Reagent preparation and sample pretreatment should be carried out in a fume hood.
When operating, wear protective equipment as required to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the liquid chromatography-triple quadrupole mass spectrometry method for the determination of omethoate, methamidophos, acephate and phoxim in water.
This standard applies to omethoate, methamidophos, acephate and phoxim in surface water, groundwater, domestic sewage and industrial wastewater.
Determination.
When the injection volume was 5.0 μl, the detection limit of the method was 0.5 μg/L, and the lower limit of determination was 2.0 μg/L. See Appendix A for details.
2 Normative references
This standard refers to the following documents or clauses thereof. For dated references, only the dated version applies to this standard.
For undated references, the latest edition (including all amendments) applies to this standard.
HJ/T 91 Technical Specification for Surface Water and Sewage Monitoring
HJ 91.1 Technical Specification for Wastewater Monitoring
HJ 164 Technical Specification for Groundwater Environmental Monitoring
3 Principles of the method
The samples were directly injected after filtration or purification, and separated and detected by liquid chromatography-triple quadrupole mass spectrometry. According to retention time and characteristic ions
Qualitative, internal standard method quantitative.
4 Interference and cancellation
4.1 When there is matrix interference in the sample, it can be reduced or eliminated by optimizing the chromatographic conditions, diluting the sample, or reducing the injection volume.
4.2 When the sample contains organic substances that interfere with the determination of the target substance, part of the interference can be removed by solid-phase extraction purification.
5 Reagents and Materials
Unless otherwise stated, analytical reagents that meet national standards were used in the analysis, and the experimental water was newly prepared without target compounds.
pure water.
5.1 Acetonitrile (CH3CN). chromatographically pure.
5.2 Methanol (CH3OH). chromatographically pure.
5.3 Ethyl acetate (CH3COOCH2CH3). chromatographically pure.
5.4 Hydrochloric acid. ρ = 1.19 g/ml, excellent grade.
5.5 Sodium Hydroxide (NaOH).
5.6 Ammonium formate (HCOONH4).
5.7 Standard products of omethoate, methamidophos, acephate, and phoxim. the purity is not less than 99.0%.
5.8 Standard products of methamidophos-d6, omethoate-d6 and phoxim-d5.the purity is not less than 99.0%.
5.9 Acetonitrile solution. φ(CH3CN) = 50%.
Mix acetonitrile (5.1) and water in a 1.1 volume ratio.
5.10 Acetonitrile-ethyl acetate mixed solution. φ(CH3CN) = 50%.
Mix acetonitrile (5.1) and ethyl acetate (5.3) in a 1.1 volume ratio.
5.11 Methanol solution. φ(CH3OH) = 80%.
Mix methanol (5.2) and water in a volume ratio of 8.2.
5.12 Hydrochloric acid solution. φ = 50%.
Hydrochloric acid (5.4) and water were mixed in a volume ratio of 1.1.
5.13 Sodium hydroxide solution. c(NaOH) = 0.1 mol/L.
Weigh 0.4 g of sodium hydroxide (5.5) and dissolve it in a small amount of water, dilute to 100 ml, and mix well.
5.14 Ammonium formate solution. c(HCOONH4) = 5.0 mmol/L.
Weigh 0.16 g of ammonium formate (5.6) and dissolve it in a small amount of water, dilute to 500 ml, and mix well.
5.15 Ammonium formate-acetonitrile solution. c = 5.0 mmol/L.
Weigh 0.16 g of ammonium formate (5.6) and dissolve it in a small amount of acetonitrile (5.1), dilute to 500 ml, and mix.
5.16 Mixed standard stock solution of omethoate, methamidophos, acephate, and phoxim. ρ = 1 000 mg/L.
Weigh 100.0 mg of omethoate, methamidophos, acephate, and phoxim standard (5.7) respectively, dissolve them in a small amount of acetonitrile (5.1).
solution, transfer to a 100 ml volumetric flask, make up to the mark with acetonitrile (5.1), and mix well. Aliquot into brown vials, seal, −15°C
The following storage in the freezer and protected from light has a shelf life of 6 months. The certified standard solution can also be directly purchased and stored according to the standard solution certificate requirements.
5.17 Mixed standard solution of omethoate, methamidophos, acephate and phoxim. ρ = 10.0 mg/L.
Pipette appropriate amount of omethoate, methamidophos, acephate, and phoxim mixed standard stock solution (5.16), dilute with acetonitrile solution (5.9)
Release, refrigerate below 4 ℃ and protect from light, the shelf life is 2 months.
5.18 Internal standard stock solution. ρ = 100 mg/L.
Weigh 10.0 mg of methamidophos-d6, omethoate-d6, and phoxim-d5 standard (5.8), dissolve with a small amount of acetonitrile (5.1), transfer to
Transfer to a 100 ml volumetric flask, make up to the mark with acetonitrile (5.1), and mix well. Dispense into brown sample vials, seal, cool below −15°C
Refrigerated and protected from light, the shelf life is 6 months. The certified standard solution can also be directly purchased and stored according to the standard solution certificate requirements.
5.19 Internal standard solution. ρ = 0.50 mg/L.
Pipette an appropriate amount of the internal standard stock solution (5.18), dilute it with acetonitrile solution (5.9), and store it under 4°C in the dark, with a shelf life of 2 months.
5.20 Solid phase extraction column I. The packing is octadecyl-bonded silica gel, or an extraction column with equivalent column efficiency, with a specification of 500 mg/6 ml.
5.21 Solid phase extraction column II. The packing is a copolymer of divinylbenzene and N-vinylpyrrolidone, or an extraction column with the same column efficiency, the specification is
500 mg/6 ml.
5.22 Filter membrane. 0.22 μm, Teflon or other equivalent material.
5.23 Nitrogen. purity ≥99.99%.
6 Instruments and equipment
6.1 Liquid chromatography-triple quadrupole mass spectrometer. equipped with electrospray ionization source (ESI).
6.2 Chromatographic column. a biphenyl chromatographic column with a particle size of 2.6 μm, a column length of 100 mm and an inner diameter of 2.1 mm, or other color with similar performance.
column.
6.3 Concentrating device. nitrogen blowing concentrator or other equipment with equivalent performance.
6.4 Amber sampling bottle. 100 ml or 250 ml screw cap glass bottle with teflon liner or ground mouth bottle with stopper.
6.5 Amber Vials. 2.0 ml screw cap glass vials with Teflon liner.
6.6 Micro syringe. 10 μl, 50 μl, 100 μl, 250 μl, 1.0 ml.
6.7 Common laboratory instruments and equipment.
7 samples
7.1 Sample Collection and Storage
Samples were collected in accordance with the relevant regulations of HJ/T 91, HJ 91.1 and HJ 164.
Use the amber sampling bottle (6.4) to collect the sample and collect the sample when the bottle is full. If the pH of the collected sample is not between 2 and 8, use a hydrochloric acid solution (5.12)
Or sodium hydroxide solution (5.13) to adjust the pH to 2-8, refrigerate below 4°C for transport and storage in the dark, and complete the sample analysis within 3 days.
7.2 Preparation of test specimens
The sample is filtered through the filter membrane (5.22), after discarding 2 ml of the primary filtrate, pipette 1.0 ml of the filtered sample into the brown sample bottle (6.5),
Add 10.0 μl internal standard solution (5.19), mix well for measurement.
Samples with complex matrices were cleaned up by solid phase extraction before injection. Take 5.0 ml of sample and pass it through at a flow rate of about 3 ml/min (about 1 drop/sec).
through a solid phase extraction cartridge. Methamidophos, omethoate and acephate were purified with solid phase extraction column I (5.20), 10 ml of acetonitrile-ethyl acetate mixed
eluted with the combined solution (5.10); phoxim was purified with solid phase extraction column II (5.21) and eluted with 10 ml of methanol (5.2). The eluates were combined and
The concentration device (6.3) is concentrated to near dryness, and the volume is made up to 5.0 ml with acetonitrile solution (5.9). After filtration through filter membrane (5.22), take 1.0 ml of
Put the solution in the brown sample bottle (6.5), add 10.0 μl of the internal standard solution (5.19), and mix well for measurement.
Note 1.If the sample concentration is high, in order to avoid saturation of the column adsorption capacity, the sample can be diluted and then purified by solid phase extraction.
Note 2.During the solid phase extraction process, if the experimental time needs to be shortened, methamidophos, omethoate and acephate can be eluted with methanol solution (5.11).
Phosphorus was eluted with methanol (5.2). Collect the eluates separately, filter them through the filter membrane (5.22), take 1.0 ml of the filtrate into the brown sample bottle (6.5),
Add 10.0 μl internal standard solution (5.19), mix well for measurement.
7.3 Preparation of blank samples
Substitute the test water for the sample, and follow the same steps as the preparation of the sample (7.2) to prepare the blank sample.
8 Analysis steps
8.1 Instrument Reference Conditions
8.1.1 Liquid chromatography reference conditions
Mobile phase A. ammonium formate solution (5.14); mobile phase B. ammonium formate-acetonitrile solution (5.15); gradient elution procedure is shown in Table 1; flow rate.
0.3 ml/min; injection volume. 5.0 μl; column temperature. 40°C.
8.1.2 Reference conditions for mass spectrometry
Positive ion mode; ionization voltage. 5 500 V; ion source temperature. 550 °C; spray gas pressure. 380 kPa; auxiliary heating gas pressure.
410 kPa; air curtain air pressure. 210 kPa; multi-ion reaction monitoring mode (MRM), see Table 2 for specific conditions.
8.1.3 Instrument tuning
There are certain differences in the tuning parameters of instruments from different manufacturers.
Calibration of instrument mass and resolution to ensure that the instrument is in the best test state.
8.2 Calibration
8.2.1 Establishment of standard curve
Pipette an appropriate amount of omethoate, methamidophos, acephate, and phoxim mixed standard working solution (5.17), dilute step by step, and prepare to
Standard series with at least 5 concentration points, the mass concentrations of each component are 0.00 μg/L, 2.00 μg/L, 5.00 μg/L, 10.0 μg/L, 50.0
100 μg/L (this is the reference concentration). Pipette 1.0 ml of the prepared standard series solution into the brown sample bottle (6.5), add 10.0 μl
Standard use solution (5.19), mix well for testing.
According to the reference conditions of the instrument (8.1), measure the standard series of solutions from low concentration to high concentration. in standard series solutions
The mass concentration (μg/L) of the standard component is the abscissa, the ratio of its corresponding peak area (or peak height) to the internal standard peak area (or peak height)
The product with the concentration of the internal standard is the ordinate, and a standard curve is established.
Note. In order to ensure uniform quantification, the solvent used in the dilution of the standard curve should be the same as the prepared sample.
8.2.2 Standard reference spectrum
Under the instrumental reference conditions (8.1) of this standard, the total ion chromatogram of the target compound (20 μg/L) is shown in Figure 1.
8.3 Sample Determination
Carry out the determination of the sample (7.2) according to the same instrumental conditions as the establishment of the standard curve (8.2.1).
8.4 Blank test
Carry out the measurement of the blank sample (7.3) according to the same instrument conditions as the sample measurement (8.3).
9 Result calculation and presentation
9.1 Qualitative Analysis
For each target compound, one precursor ion and two product ions were selected for qualitative analysis. Under the same experimental conditions, the target in the sample
Compare the retention time of the compound with the retention time of the target compound in the standard sample, and the absolute value of the relative deviation should be less than 2.5%; the sample spectrum
The relative ion abundance (Ksam) of the qualifier ions of each target compound in the figure is similar to the phase of the corresponding qualifier ions in the standard solution spectrum of which the concentration is close.
Comparing the ion abundance (Kstd), if the deviation does not exceed the range specified in Table 3, it can be determined that the corresponding target compound exists in the sample.
9.3 Result representation
The retention of the number of digits after the decimal point of the determination result is consistent with the detection limit of the method, and a maximum of 3 significant figures are retained.
10 Accuracy
10.1 Precision
Six laboratories performed six replicates of surface water samples spiked with target compounds at concentrations of 2.0 µg/L and 20.0 µg/L. Experimental
The indoor relative standard deviations were 1.7%-16%, 1.9%-20%; the inter-laboratory relative standard deviations were 6.0%-18%, 3.2%-
10%; repeatability limits are 0.3 μg/L～0.5 μg/L, 2.5 μg/L～5.3 μg/L; reproducibility limits are 0.5 μg/L～1.0 μg/L,
3.6 μg/L～7.0 μg/L.
Groundwater samples spiked with target compounds at 2.0 µg/L and 20.0 µg/L were measured in 6 replicates by 6 laboratories. Experimental
The indoor relative standard deviations were 1.6%-14%, 1.5%-18%; the inter-laboratory relative standard deviations were 7.8%-11%, 4.5%-
16%; repeatability limits are 0.2 μg/L～0.5 μg/L, 3.3 μg/L～5.4 μg/L; reproducibility limits are 0.5 μg/L～0.6 μg/L,
5.5 μg/L～9.5 μg/L.
Six laboratories performed six replicate determinations of domestic sewage samples spiked with target compounds at concentrations of 2.0 µg/L and 20.0 µg/L.
The intra-laboratory relative standard deviations were 2.1%-19%, 1.2%-17%; the inter-laboratory relative standard deviations were 9.6%-17%,
3.2%～17%; repeatability limits are 0.3 μg/L～0.5 μg/L, 3.3 μg/L～6.1 μg/L; reproducibility limits are 0.7 μg/L～
0.9 µg/L, 3.4 µg/L～9.3 µg/L.
Total outflow samples of organophosphorus production wastewater spiked with target compounds at concentrations of 2.0 µg/L, 20.0 µg/L and.200 µg/L from 6 laboratories
Six replicate determinations were performed. the intra-laboratory relative standard deviations were 3.5% to 19%, 1.7% to 20%, and 2.8% to 14%;
The relative standard deviations were 4.7%-17%, 4.1%-14%, 4.0%-12%, respectively; the repeatability limits were 0.3 µg/L-0.6 µg/L,
4.5 µg/L～6.0 µg/L, 29 µg/L～45 µg/L; reproducibility limits are 0.6 µg/L～1.0 µg/L, 4.7 µg/L～8.7 µg/L, 36 µg/L～
72 µg/L.
The 6 laboratories have treated the organic phosphorus production wastewater containing the average concentration of methamidophos at 1.3 µg/L and the average concentration of acephate at 1.5 µg/L.
The inter-laboratory samples were repeatedly determined for 6 times. the intra-laboratory relative standard deviation was 3.7%-19%; the inter-laboratory relative standard deviation was
6.3%～7.5%; repeatability limit is 0.4 µg/L～0.6 µg/L; reproducibility limit is 0.5 µg/L～0.6 µg/L.
The 6 laboratories have treated the organic phosphorus production wastewater containing the average concentration of methamidophos at 1.3 µg/L and the average concentration of acephate at 1.5 µg/L.
The samples from the inter-drainage outlet were spiked at 2.0 µg/L and 20.0 µg/L, respectively, and six repeated determinations were carried out. the relative standard deviations in the laboratory were 1.4%～
16%, 0.93%-15%; the relative standard deviations between laboratories were 2.3%-13%, 6.0%-12%; the repeatability limits were 0.4 µg/L-
0.7 µg/L, 2.6 µg/L～4.2 µg/L; the reproducibility limits are 0.5 µg/L～0.8 µg/L, 4.9 µg/L～7.1 µg/L, respectively.
10.2 Correctness
Six laboratories performed six analytical determinations on surface water samples spiked with target compounds at concentrations of 2.0 µg/L and 20.0 µg/L.
The standard recovery rates were 69.8%～110%, 72.8%～110%, and the final values of the standard addition recoveries were (91.8±33.8)%～(99.3±13.2)%,
(87.3±18.2)%～(104±10.0)%.
Six laboratories performed six analytical determinations on groundwater samples spiked with target compounds at concentrations of 2.0 µg/L and 20.0 µg/L.
The standard recovery rates were 77.4%-115%, 68.6%-114%, and the final values of the standard addition recoveries were (86.0±14.4)%-(103±16.2)%,
(91.3±22.0)%～(99.8±18.2)%.
Six laboratories carried out six analytical determinations on domestic sewage samples spiked with target compounds at concentrations of 2.0 µg/L and 20.0 µg/L.
The recovery rates of standard addition were 70.1%～110%, 68.8%～109%, and the final values of standard addition recoveries were (90.0±26.0)%～
(94.0±18.2)%, (88.5±24.0)%～(94.7±6.0)%.
Total outflow samples of organophosphorus production wastewater spiked with target compounds at concentrations of 2.0 µg/L, 20.0 µg/L and.200 µg/L from 6 laboratories
Six analytical determinations were carried out. the recovery rates of standard addition were 67.2% to 110%, 72.8% to 110%, and 79.2% to 110%, and the recovery rate of standard addition was the highest.
The final values were (90.5±26.0)%～(99.8±9.4)%, (88.3±16.0)%～(100±8.2)%, and (90.2±13.2)%～(98.2±7.8)%, respectively.
The 6 laboratories have treated the organic phosphorus production wastewater containing the average concentration of methamidophos at 1.3 µg/L and the average concentration of acephate at 1.5 µg/L.
The samples were spiked with 2.0 µg/L and 20.0 µg/L for 6 times, respectively, and the recovery rates were 70.2%-112%,
67.2%～110%, and the final recovery rates of standard addition were (88.1±20.0)%～(105±13.0)%, (84.7±22.0)%～(101±22.0)%.
See Appendix B for the precision and correctness results statistics.
11 Quality Assurance and Quality Control
11.1 Blank test
Every 20 samples or each batch (less than 20 samples) should do at least one blank test, and the determination result should be lower than the detection limit of the method.
11.2 Calibration
Before analyzing the sample, a standard curve should be established that can cover at least 5 concentration points of the sample concentration range, and the correlation coefficient of the curve should be ≥
0.995.Every 20 samples or each batch (less than 20 samples) should be determined at an intermediate concentration point of the standard curve, and its determination result is consistent with the standard
The relative error of the concentration at this point of the curve should be within ±20%, otherwise, a new standard curve should be established.
11.3 Parallel samples
Every 20 samples or each batch (less than 20 samples) should analyze a parallel sample, and the relative deviation of the parallel samples in the laboratory should be ≤20%.
11.4 Matrix spikes
Analysis of one matrix spike should be performed every 20 samples or batches (less than 20 samples), and the matrix spike recovery should be within
Between 60% and 130%.
12 Waste Disposal
The waste generated in the experiment should be collected centrally, marked accordingly, and entrusted to a qualified unit for disposal according to law.
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