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Food safety national standard -- Determination of 20 Pesticide Residues in Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry
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GB 23200.37-2016
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Basic data | Standard ID | GB 23200.37-2016 (GB23200.37-2016) | | Description (Translated English) | Food safety national standard -- Determination of 20 Pesticide Residues in Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 18,158 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2323-2009 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration |
GB 23200.37-2016: Food safety national standard -- Determination of 20 Pesticide Residues in Foods by Liquid Chromatography-Mass Spectrometry / Mass Spectrometry ---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.
Food safety national standard - Determination of 20 Pesticide Residues in Foods by Liquid Chromatography-Mass Spectrometry/Mass Spectrometry
Instead of SN/T 2323-2009
National standards for food safety
Food in the acid insecticides, dinduazins and other 20 kinds of pesticides
Determination of residual amount
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of residue of 20 pesticides including nitenpyram, dinotefuran etc in
Foods
Liquid chromatography - tandem mass spectrometry
200 × - × - × release
200 × - × - × implementation
National Health and Family Planning Commission of the People 's Republic of China
Issued by the Ministry of Agriculture of the People 's Republic of China
State Administration of Food and Drug Administration
GB
National Standards of People's Republic of China
2016-12-18 Release.2017-06-18 Implementation
Foreword
This standard replaces SN/T 2323-2009 "20 kinds of pesticide residues in the import and export of food insects, dinotech and other pesticide residues detection method liquid color
Spectrum-mass spectrometry/mass spectrometry ".
Compared with SN/T 2323-2009, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name of the "export food" to "food";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 2323-2009.
National standards for food safety
Determination of 20 Pesticide Residues in Foods
Liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the food in the dienetraxine, dinotefuran, spiramycin, butylbenzene morpholine, acaricidomide - formamidine, thiophosphate,
Acarbidomide, metoclopramide, polymycamycin A, polymycamycin D, aminobiomycin, methylaminobiomycin 1, methylamino
Abamectin 2, allyl grass chloride, deworming phosphorus, diniconazole, abamectin, aminoside amikacin pesticide residues liquid chromatography-mass spectrometry
/ Mass spectrometry method and sample preparation method.
This standard applies to the import and export of rice, brown rice, corn, barley and wheat in the above 20 kinds of pesticide residues detection and confirmation, the other
Food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article
Pieces. For undated references, the latest edition (including all modifications) applies to this document.
GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs
GB/T 6682 Analytical laboratory water specifications and test methods
3 principle
The samples were extracted with aqueous acetonitrile and partitioned with n-hexane liquid, followed by graphite carbon and N-propyl ethylenediamine solid phase extraction (PSA)
And identified by liquid chromatography-mass spectrometry/mass spectrometer and quantified by external standard method.
4 reagents and materials
Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 n-hexane (C6H14).
4.1.2 Toluene (C7H8).
4.1.3 Methanol (CH4O).
4.1.4 Acetonitrile (C2H3N).
4.1.5 Formic acid (CH2O2).
4.1.6 Sodium chloride (NaCl). Analytical purity.
4.1.7 magnesium sulfate heptahydrate (MgSO4 · 7H2O). analytical grade.
4.2 solution preparation
4.2.1 acetonitrile-toluene solution (3 1, V/V). take 300 mL of acetonitrile, add 100 mL of toluene, shake back.
4.3 standards
4.3.1 Pesticide Standards. Nitenpyram, CAS No.. 150824-47-8, Dinotefuran, CAS No..165252-70-0,
Spiroxamine, CAS No..118134-30-8, Fenpropimorph (CAS No..67564-91-4), acaricidal-
(Diafenthiuron-methanimidamide, CAS No..136337-81-9), trismorpholine (Tridemorph, CAS No..81412-43-3),
Metconazole, CAS No..125116-23-6, Diafenthiuron-urea, CAS No..136337-67-2,
(Spinosyn A, CAS No..131929-60-7), polymyxin D (Spinosyn D, CAS No..131929-63-0), allyl chloride
(Dichlormid, CAS No..37764-25-3), insecticidal phosphorus (Naphthalophos, CAS No..1491-41-4), diniconazole,
CAS No..83157-10-3) purity ≥97%; Milbemectin (CAS No.. 51596-10-2), Tiamulin-fumarate,
CAS No..55297-96-6), Emamectin-amino, Emamectin-methylamino 1,
(Amamectin-methylamino 2), abamectin (CAS No..71751-41-2), methyl formic acid amide
The purity of Emamectin-N-methyl formyl amino was more than 80%.
4.4 standard solution preparation
4.4.1 standard reserve solution. respectively, accurately weighed the right amount of pesticide standards, with acetone dubbed the concentration of 100 μg/mL standard stock solution.
The standard stock solution is stored at 0 ° C to 4 ° C and is prepared every 12 months.
4.4.2 mixed standard stock solution. respectively, to absorb the right amount of close to Ting, tiamulin, polymycamycin A, polymycamycin D, amino averae
1, methionine avermectin 2, allyl grass chloride, insecticidal phosphorus, diniconazole, abamectin, methyl formate Ave
The standard stock solution of the 12 kinds of pesticides was mixed into a standard stock solution for the A group of pesticides, the concentration of the mixed standard stock solution was 10
Μg/mL, respectively, to absorb the appropriate amount of allyl insects, dinotefuran, spirocosporin, butylbenzene morpholine, acaricidomide - formamidine, thiophosphate,
The eight standard mixed stock solutions of the acaricidon-urea were mixed into a standard stock solution for the concentration of the B group of pesticides and the mixed standard stock solution
For 10 μg/mL. The standard stock solution is stored at 0 ° C to 4 ° C and is prepared every 6 months.
4.4.3 mixed standard working solution. A group and B group of pesticide mixed standard stock solution were diluted with acetonitrile to the appropriate concentration of standard workers
For liquid. In 0 ℃ ~ 4 ℃ under the conditions of storage. Prepared once every 3 months.
5 instruments and equipment
5.1 High Performance Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Rotary Evaporator.
5.4 Oscillator.
5.5 Centrifuge. 5 000 r/min.
5.6 solid phase extraction column. graphite carbon/N-propyl ethylenediamine (PSA), 6 mL, 500 mg/500 mg, or equivalent.
5.7 with a plugged mouth Erlenmeyer flask. 300 mL.
5.8 Centrifuge tube. 50 mL, plastic.
5.9 Filtration. 0.45 μm, organic phase.
6 Preparation and storage of samples
Take rice, brown rice, corn, barley and wheat and other representative samples of about 500 g, the sampling site according to GB 2763 Appendix A, with powder
Crushed into a clean container, sealed and marked. 4 ℃ below the preservation.
7 Analysis steps
7.1 Extraction
Weigh the sample 20 g (accurate to 0.1 g) in a 300 mL stoppered Erlenmeyer flask and add 30 mL of water for 30 min. Join
80 mL of acetonitrile, shaken for 30 min, the supernatant 30 mL placed in 50 mL plastic centrifuge tube, add 3 g magnesium sulfate, 2 g sodium chloride and 10 mL
N-hexane, shake 5 min, 3 000 r/min centrifugal 5 min, accurate removal of the middle layer (acetonitrile layer) 10 mL, for purification.
7.2 Purification
The graphite carbon/ethylenediamine propyl solid phase extraction column was pre-leached with 10 mL of acetonitrile in toluene and the 10 mL of acetonitrile solution
The samples were loaded onto a solid phase extraction column (SPE) and the effluent was collected. Eluting with 30 mL of acetonitrile in toluene, collecting the eluate, collecting the solution,
Concentrated in a 40 ° C water bath under reduced pressure to dryness, and the residue was separated with 1 mL of methanol and the membrane was measured and confirmed by liquid chromatography-mass spectrometry/mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
A) Column. C18,5 μm, 150 x 2.1 mm (inner diameter), or equivalent;
B) mobile phase. mobile phase A is acetonitrile, B is 0.1% formic acid aqueous solution, gradient elution program in Table 1;
C) Flow rate. 300 μL/min;
D) Injection volume. 30 μL for group A; 20 μL for group B.
Table 1 gradient elution program
7.3.2 Mass spectrometry reference conditions
Group A Pesticide Group B Pesticides
Time (min)
Mobile phase ratio
Time (min)
Mobile phase ratio
ABAB
9 65 35 2 30 70
9.1 95 5 5 40 60
15.1 25 75 14 95 5
19 25 75 14.1 15 85
A) ion source. electrospray ion source;
B) Scanning mode. positive ion scanning;
C) Detection method. Multiple reaction monitoring (MRM);
D) atomization gas, air curtain gas, auxiliary gas, collision gas are high purity nitrogen; before using the parameters to adjust the mass spectrometry sensitivity to detect
For reference, see Appendix A.
7.3.3 Determination and confirmation of chromatography
According to the content of the sample in the sample, select the mixed standard working solution with similar response value for chromatographic analysis. Mixed standard working fluid
And the response value of the pesticide in group A and group B of the test solution should be within the linear response range of the instrument. A group of mixed standard working fluid and sample solution, B
Group of mixed standard working fluid and sample solution volume measurement. In the above liquid chromatography-mass spectrometry/mass spectrometry conditions, the A group of pesticides were retained
(Min). minocarmin 1.8, tiamulin 4.5, polymycamycin A 8.0, polymycamycin D 8.5, aminobiomycin 8.9, a
Aminobirobi 1 9.0, methylamino averobacter 2 9.3, allyl chloride 10.5, insect repellent phosphorus 11.7, diniconazole 13.5, avermectin 16.0,
Methicillin Avermectin 16.2; Group B pesticide retention time is about (min). alkenolone 2.0, dinotefuran 2.5, spirocosamine 8.1,
Butylbenzene morphine 8.1, acaricidal-formamidine 9.5, thiophanate 9.7, phytosezide 13.0, acaricidal-urea 14.6. Standard mass spectrometry of the standard solution
The multi-reaction monitoring mass chromatogram is given in Appendix B.
The sample was determined according to the above liquid chromatography-mass/mass spectrometry conditions. If the retention time of the chromatographic peak of the test sample was consistent with that of the standard, and
And the concentration of the standard working solution of the relative abundance of consistent, relative abundance tolerance does not exceed the range specified in Table 2, you can determine the sample
There is a corresponding measured object.
Table 2 qualitatively confirms the maximum allowable deviation of relative ion abundance
Relative ion abundance 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.4 blank test
In addition to the sample, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processor or according to formula (1) to calculate the content of various pesticides in the sample, the calculation results need to deduct the blank value.
A × c × V
AS x m
Where. X - the amount of pesticide in the sample, micrograms per kilogram, μg/kg;
C - the concentration of pesticide in the standard working fluid, in ng/ml for ng/ml;
A - peak area of pesticide in sample solution;
AS - standard working area of pesticide peak area;
V - the final volume of the sample solution, in milliliters, mL;
M - the amount of sample represented by the final sample, in grams, g;
Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix D requirements.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix E requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification was 5 μg/kg.
10.2 Recovery rate
X = (1)
See Appendix C for the recovery rate.
Appendix A1)
(Informative)
Mass spectrometry conditions
A) electrospray voltage (IS). 5.200 V;
B) Atomizing gas pressure (GS1). 50 psi;
C) air curtain gas pressure (CUR). 15 psi;
D) Auxiliary gas pressure (GS2). 30 psi;
E) ion source temperature (TEM). 670 C;
F) collision gas (CAD). 12;
G) qualitative ion pairs of 20 pesticides, quantitative ion pair, Dwell time, de-cluster voltage (DP), inlet voltage
(EP), collision energy (CE) and collision chamber outlet voltage (CXP) parameters are shown in Table A.1.
Table A.1 Qualitative ion pairs, quantitative ion pairs and mass spectral parameters
Component name
Qualitative ion pair
M/z
Quantitative ion pair
M/z
Dwell time
(Dwell
Time/ms
To cluster voltage
(DP)/V
Inlet voltage
(EP)/V
Collision energy
(CE)/V
Collision chamber exit
Voltage (CXP)
/ V
Enamidophos
271.2/98.8
271.2/98.8
271.2/196.1 100 30 6 25 18
Dinotech
203.0/129.0
203.0/129.0
203.0/87.0 100 23 6 22 8
Spiramine
298.4/144.1
298.4/144.1
100 60 13 29 13
298.4/99.9 100 60 13 45 18
Butylbenzene
304.3/147.0
304.3/147.0
304.3/97.8 100 60 4 43 11
Acaricidal-formamidine
353.3/297.4
353.3/297.4
353.3/280.1 100 60 8 36 17
Thirteen morpholine
298.4/130.1
298.4/130.1
298.4/97.8 100 60 10 39 18
Phytosex
320.2/69.7
320.2/69.7
320.2/124.8 100 57 8 50 10
Acarbide-urea
369.2/229.0
369.2/229.0
369.2/271.3 100 60 9 30 20
Close
510.4/207.9
510.4/207.9
510.4/190.4 150 40 6 30 14
Tiamectin
494.3/192.3
494.3/192.3
100 106 10 32 14
494.3/163.4 100 50 10 44 9
Methicillin A
732.5/142.1
732.5/142.1
732.5/189.0 100 55 8 47 11
Polymycin D
746.4/142.1
746.4/142.1
100 50 13 45 15
746.4/189.1 100 50 13 45 15
Aminobiose
872.6/144.1
872.6/144.1
872.6/256.0 100 60 8 38 15
Methylamino avi
886.6/158.2
886.6/158.2
100 55 11 50 14
886.6/82.3 100 55 10 120 14
Methylamino avi
886.6/158.2
886.6/158.2
100 55 11 50 14
886.6/82.3 100 55 10 120 14
Allylamide
208.1/97.8
208.1/97.8
208.1/139.9 100 30 9 18 7
Pest insects
350.2/214.2
350.2/214.2
350.2/276.0 100 55 7 30 16
Diniconazole
326.2/69.7
326.2/69.7
326.2/159.1 100 60 8 47 12
Avermectin
896.6/186.4
896.6/186.4
896.6/154.2 150 90 5 44 11
Methyl formate
Avermectin
914.6/186.2
914.6/186.2
150 50 10 45 10
914.6/153.8 150 50 10 50 10
1) The parameters listed in Appendix A are done on the API4000 mass spectrometer, where the experimental instrument model is listed for reference only and does not involve commercial purposes.
Users try to use different manufacturers and models of equipment.
Appendix B
(Informative)
Standard Quality Chromatogram
XIC of MRM (22 pairs). 510.4/207.9 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.8040.0 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
2.0e5
4.0e5
6.0e5
8.0e5
1.0e6
1.2e6
1.4e6
1.6e6
1.8e6
2.0e6
2.2e6
2.4e6
2.6e6
2.8e6
3.0e6
3.2e6
3.4e6
3.6e6
In
Te
Ns
Ity
, C
Ps
5.083.92
Figure B.1 Group A Pesticide Standard Multi-Reaction Monitoring Total Ion Flow Chart (XIC)
1, secreptin 2, tiamulin 3, polymycamycin A 4, polymycamycin D 5, aminobiomulin 6, methylaminobiomycin 1
7, methylamino abamectin 2 8, allyl grass amine 9, insect repellent phosphorus 10, diniconazole 11, avermectin 12, amoxycarbamate
XIC of MRM (22 pairs). 510.4/207.9 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.8040.0 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
Inte
Nsit
Y, c
Ps
5.08
3.92
XIC of MRM (22 pairs). 510.4/190.4 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.5760.0 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
Inte
Nsit
Y, c
Ps
3.97
XIC of MRM (22 pairs). 494.3/192.3 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.6.4e5 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
5.0e4
1.0e5
1.5e5
2.0e5
2.5e5
3.0e5
3.5e5
4.0e5
4.5e5
5.0e5
5.5e5
6.0e5
6.4e5
Inte
Nsit
Y, c
Ps
3.91
XIC of MRM (22 pairs). 494.3/163.4 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.2e5 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.00
5000.00
1.00e4
1.50e4
2.00e4
2.50e4
3.00e4
3.50e4
4.00e4
4.50e4
5.00e4
5.50e4
6.00e4
6.50e4
7.00e4
7.50e4
8.00e4
8.50e4
9.00e4
9.50e4
1.00e5
1.05e5
1.10e5
1.15e5
1.20e5
1.24e5
Inte
Nsit
Y, c
Ps
3.92
510.4/190.4
510.4/207.9
494.3/192.3
494.3/163.4
Close
Tiamectin
Close
Tiamectin
XIC of MRM (22 pairs). 732.5/142.1 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.3.6e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
2.0e5
4.0e5
6.0e5
8.0e5
1.0e6
1.2e6
1.4e6
1.6e6
1.8e6
2.0e6
2.2e6
2.4e6
2.6e6
2.8e6
3.0e6
3.2e6
3.4e6
3.6e6
Inte
Nsit
Y, c
Ps
8.03
XIC of MRM (22 pairs). 732.5/189.0 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.1e5 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.00
5000.00
1.00e4
1.50e4
2.00e4
2.50e4
3.00e4
3.50e4
4.00e4
4.50e4
5.00e4
5.50e4
6.00e4
6.50e4
7.00e4
7.50e4
8.00e4
8.50e4
9.00e4
9.50e4
1.00e5
1.05e5
1.08e5
Inte
Nsit
Y, c
Ps
8.02
XIC of MRM (22 pairs). 746.4/142.1 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.3.0e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
2.0e5
4.0e5
6.0e5
8.0e5
1.0e6
1.2e6
1.4e6
1.6e6
1.8e6
2.0e6
2.2e6
2.4e6
2.6e6
2.8e6
3.0e6
Inte
Nsit
Y, c
Ps
8.47
XIC of MRM (22 pairs). 746.4/189.1 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.2e5 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.00
5000.00
1.00e4
1.50e4
2.00e4
2.50e4
3.00e4
3.50e4
4.00e4
4.50e4
5.00e4
5.50e4
6.00e4
6.50e4
7.00e4
7.50e4
8.00e4
8.50e4
9.00e4
9.50e4
1.00e5
1.05e5
1.10e5
1.15e5
1.20e5
Inte
Nsit
Y, c
Ps
8.47
XIC of MRM (22 pairs). 872.6/144.1 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.8.2e5 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
5.0e4
1.0e5
1.5e5
2.0e5
2.5e5
3.0e5
3.5e5
4.0e5
4.5e5
5.0e5
5.5e5
6.0e5
6.5e5
7.0e5
7.5e5
8.0e5
Inte
Nsit
Y, c
Ps
8.87
9.19
XIC of MRM (22 pairs). 872.6/256.0 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.6e4 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1000.0
2000.0
3000.0
4000.0
5000.0
6000.0
7000.0
8000.0
9000.0
1.0e4
1.1e4
1.2e4
1.3e4
1.4e4
1.5e4
1.6e4
Inte
Nsit
Y, c
Ps
8.87
XIC of MRM (22 pairs). 886.6/158.2 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.2.0e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1.0e5
2.0e5
3.0e5
4.0e5
5.0e5
6.0e5
7.0e5
8.0e5
9.0e5
1.0e6
1.1e6
1.2e6
1.3e6
1.4e6
1.5e6
1.6e6
1.7e6
1.8e6
1.9e6
2.0e6
Inte
Nsit
Y, c
Ps
9.00
9.31
732.5/142.1
732.5/189.0
746.4/142.1
746.4/142.1
872.6/144.1
872.6/256.0
886.6/158.2
Methicillin A
Methicillin A
Polymycin D
Polymycin D
Aminobearin
Aminobearin
Methicillin 1
XIC of MRM (22 pairs). 886.6/82.3 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.2e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.00
5.00e4
1.00e5
1.50e5
2.00e5
2.50e5
3.00e5
3.50e5
4.00e5
4.50e5
5.00e5
5.50e5
6.00e5
6.50e5
7.00e5
7.50e5
8.00e5
8.50e5
9.00e5
9.50e5
1.00e6
1.05e6
1.10e6
1.15e6
1.20e6
Inte
Nsit
Y, c
Ps
9.00
9.31
XIC of MRM (22 pairs). 886.6/158.2 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.2.0e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1.0e5
2.0e5
3.0e5
4.0e5
5.0e5
6.0e5
7.0e5
8.0e5
9.0e5
1.0e6
1.1e6
1.2e6
1.3e6
1.4e6
1.5e6
1.6e6
1.7e6
1.8e6
1.9e6
2.0e6
Inte
Nsit
Y, c
Ps
9.00
9.31
XIC of MRM (22 pairs). 886.6/82.3 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.2e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.00
5.00e4
1.00e5
1.50e5
2.00e5
2.50e5
3.00e5
3.50e5
4.00e5
4.50e5
5.00e5
5.50e5
6.00e5
6.50e5
7.00e5
7.50e5
8.00e5
8.50e5
9.00e5
9.50e5
1.00e6
1.05e6
1.10e6
1.15e6
1.20e6
Inte
Nsit
Y, c
Ps
9.00
9.31
XIC of MRM (22 pairs). 208.1/97.8 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.3e4 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
500.0
1000.0
1500.0
2000.0
2500.0
3000.0
3500.0
4000.0
4500.0
5000.0
5500.0
6000.0
6500.0
7000.0
7500.0
8000.0
8500.0
9000.0
9500.0
1.0e4
1.1e4
1.1e4
1.2e4
1.2e4
1.3e4
1.3e4
Inte
Nsit
Y, c
Ps
10.48
XIC of MRM (22 pairs). 208.1/139.9 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.4e4 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1000.0
2000.0
3000.0
4000.0
5000.0
6000.0
7000.0
8000.0
9000.0
1.0e4
1.1e4
1.2e4
1.3e4
1.4e4
Inte
Nsit
Y, c
Ps
10.48
XIC of MRM (22 pairs). 350.2/214.2 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.2.7e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1.0e5
2.0e5
3.0e5
4.0e5
5.0e5
6.0e5
7.0e5
8.0e5
9.0e5
1.0e6
1.1e6
1.2e6
1.3e6
1.4e6
1.5e6
1.6e6
1.7e6
1.8e6
1.9e6
2.0e6
2.1e6
2.2e6
2.3e6
2.4e6
2.5e6
2.6e6
2.7e6
Inte
Nsit
Y, c
Ps
11.65
XIC of MRM (22 pairs). 350.2/276.0 amu from Sample 2 (50 ng/mL) of part A. wiff (Turbo Spray) Max.1.4e6 cps.
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
Time, min
0.0
1.0e5
2.0e5
3.0e5
4.0e5
5.0e5
6.0e5
7.0e5
8.0e5
9.0e5
1.0e6
1.1e6
1.2e6
1.3e6
1.4e6
Inte
Nsit
Y, c
Ps
1...
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