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GB 23200.90-2016: Food safety national standard -- Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry
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Food safety national standard -- Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry
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GB 23200.90-2016
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Basic data | Standard ID | GB 23200.90-2016 (GB23200.90-2016) | | Description (Translated English) | Food safety national standard -- Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 18,195 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 3156-2012 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.90-2016: Food safety national standard -- Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry
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Food safety national standard - Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry
National standards for food safety
Milk and dairy products in a variety of carbamate pesticide residues
The amount of the determination
Liquid chromatography - mass spectrometry
National food safety standards-
Determination of multiple carbamate pesticides residues in milk and dairy products
Liquid chromatography - mass spectrometry
Replace SN/T 3156-2012
2016-12-18 release
2017-06-18 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
Foreword
This standard replaces SN/T 3156-2012 "Determination of various carbamate pesticide residues in milk and dairy products Liquid Chromatography - String
Combined mass spectrometry ".
Compared with SN/T 3156-2012, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- "Other food can be referred to in the standard range";
This standard replaced the previous version of the standard release.
-SN/T 3156-2012.
National standards for food safety
Determination of various carbamate pesticide residues in milk and dairy products
Liquid chromatography - mass spectrometry
1 Scope
This standard provides milk and dairy products in the kill line Wei, methomyl, pirimicarb, aldicaril, speed off Granville, evil worms, grams of Budweiser,
Determination of 14 kinds of carbamate pesticide residues by flow cytometry-mass spectrometry
Detection method.
This standard applies to pure milk, yogurt, milk powder, cheese and fruit milk in the kill line Wei, Dudu Wei, pirimicarb, aldicarb,
Determination and confirmation of residual residues of carbamazepine, carbofuran, furosemide, isoprocarb, methacillin, sec.
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 acetonitrile, and the extract was purified by solid phase extraction column and eluted with methanol. The samples were detected and confirmed by liquid chromatography-tandem mass spectrometry.
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 acetonitrile (C2H3N). residual grade.
4.1.2 Methanol (CH4O). Residue.
4.1.3 formic acid (CH2O2). excellent grade pure.
4.1.4 methanol - water solution (3 2, V/V). accurate measurement of 60 mL of methanol and 40 mL of water, mixed with spare.
4.1.5 anhydrous sodium sulfate (Na2SO4). analysis of pure, by 650
OC burning 4 h, stored in a sealed container in reserve.
4.1.6 Sodium chloride (NaCl). Analytical purity.
4.2 standards
4.2.1 Pesticide standard substances. kill line Wei, methomyl, pirimicarb, aldicarb, speed off Granville, evil worm Granville, grams of Budweiser, carnoside,
Isoprocarbamate, methamidium, Zhong Dingwei, the killing of Granville and a sulfur Granville, purity ≥ 98.5%. Refer to Appendix A for reference material information.
4.3 standard solution preparation
4.3.1 standard stock solution. accurately weighed appropriate amount of various carbamate standard material, with methanol prepared into a concentration of 100 μg/mL
Of the standard stock solution, -18 oC preservation.
4.3.2 mixed standard intermediate solution. respectively, accurately absorb the appropriate amount of carbamate pesticide standard stock solution, with methanol prepared into the concentration of
5 μg/mL mixed standard intermediate solution, -18 oC stored.
4.3.3 matrix mixed standard working solution. according to the need to absorb the appropriate amount of mixed standard intermediate solution, with a blank sample matrix solution prepared into appropriate
When the concentration of the standard working solution mixed, 0 ~ 4 oC refrigerator to save, use before the preparation.
4.4 Materials
4.4.1 Microporous membrane. 13 mm × 0.22 μm, organic.
4.4.2 C18 solid phase extraction column. ENVI
TM-181) 1 000 mg, 6 mL, or equivalent.
5 instruments and equipment
5.1 Liquid Chromatography - Tandem Mass Spectrometer. Equipped with an electrospray ion source (ESI).
5.2 Balance. 0.01 g and 0.0001 g.
5.3 Homogenizer.
5.4 Centrifuge. 4 000 r/min.
5.5 Rotary evaporator.
5.6 Polypropylene centrifuge tube. 50 mL.
5.7 Flasks. 100 mL.
6 sample preservation
Pure milk, yogurt, fruit milk, cheese is equal to 0 ~ 4 oC preservation, milk powder sealed at room temperature.
7 Analysis steps
7.1 Extraction
7.1.1 pure milk, yogurt, fruit milk, cheese and so on
Weigh the sample 5 g (accurate to 0.01 g) in 50 mL centrifuge tube, add 20 mL of acetonitrile and 5 g of anhydrous sodium sulfate,
Quality extraction 1 min, adding 2 g sodium chloride, oscillation, centrifugation at 4 000 r/min 3 min. Take the supernatant and remove 10 mL of the residue
Acetonitrile repeated extraction 1 times, combined supernatant, 40 o C water bath in the rotary evaporation concentrated to near dry, add 5 mL of methanol dissolved to be purified.
7.1.2 milk powder and so on
Weigh the sample 3 g (accurate to 0.01 g) in 50 mL centrifuge tube, add 5 mL of water, 30 o C water bath for 10 min. again
Add 20 mL of acetonitrile and 5 g of anhydrous sodium sulfate, homogenously extracted 1 min, adding 2 g of sodium chloride, shaking at 4 000 r/min
Centrifuge 3 min. The supernatant was taken and the residue was extracted again with 10 mL of acetonitrile. The supernatant was combined and rotated in a 40 o C water bath
Evaporation concentrated to near dry, add 3 mL of methanol dissolved to be purified.
7.2 Purification
After activation of ENVI-18 solid phase extraction with 10 mL of methanol, the active solution was discarded and the 2 mL extract was taken. With 15 mL of methanol
Perform elution (flow rate no more than 1 mL/min). Collect the sample and the entire eluent in a 100 mL flask and rotate in a 40 o C water bath
Evaporate to near dryness. Dry with nitrogen, methanol - water solution (3 2, V/V) dissolved and fixed to 1.0 mL, filter membrane for liquid phase color
Determination and confirmation of spectrum - tandem mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
A) Column. Thermo Hypersil GOLD C18, 150 mm × 2.1 mm (id), 5 μm, or equivalent;
B) Column temperature. 30 oC;
1) ENVITM-18 solid phase extraction column is SUPELCO company's product name, given this information is to facilitate the standard of the user, not to show
The approval of the product, if other equivalent products have the same effect, you can use these equivalent products.
C) Flow rate. 0.25 mL/min;
D) Injection volume. 10 μL;
E) Flow phase and gradient elution conditions are shown in Table 1.
Table 1 Mobile phase and gradient elution conditions
time
(Min)
Flow rate
(ΜL/min)
Methanol
(%)
0.1% formic acid aqueous solution
(%)
0.00 250 30.0 70.0
1.00 250 40.0 60.0
2.00 250 60.0 40.0
3.00 250 80.0 20.0
5.00 250 95.0 5.0
9.00 250 95.0 5.0
9.10 250 30.0 70.0
12.00 250 30.0 70.0
7.3.2 Mass spectrometry reference conditions
A) ionization mode. electrospray ionization (ESI);
B) Scanning mode. positive ion scanning;
C) Detection method. Multiple reaction monitoring (MRM);
D) electrospray voltage. 4.2 kV;
E) sheath gas, auxiliary gas are high purity nitrogen, collision gas for high purity argon. Before use, adjust the gas flow to make mass spectrometry sensitivity
To meet the testing requirements;
F) ion source temperature. 350 C;
G) Qualitative ion pairs, quantitative ion pairs, lens compensation voltage and collision energy and other parameters see Appendix A.
7.3.3 Determination and confirmation of chromatography
According to the sample content of the sample, the selected concentration of similar matrix mixed standard working solution, matrix mixed standard working solution and to be
The response values of 14 carbamate pesticides in the sample solution should be within the linear range of the instrument. Matrix mixed standard working solution and sample solution
Determination of volume by volume. For more information on the multi-reaction monitoring (MRM) chromatograms of 14 carbamate pesticide standards, see Appendix B.
The standard solution and sample solution are determined according to the conditions specified in 7.3.1 and 7.3.2. If the same retention time as the standard solution in the sample solution is
Peak appears, then its confirmation. The results show that the retention time of the chromatographic peaks is consistent with that of the reference material, and after deducting the background
The selected ions are present; the abundance of the selected ions is greater than the relative abundance of the ions associated with the standard sample
Caused by similarity within the allowable deviation (see Table 2), you can determine the existence of the corresponding sample in the sample. Using the standard curve of the matrix solution
Quantitative method.
Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation
Relative ion abundance > 50% > 20% to 50% > 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.4 blank test
Unless the sample is not weighed, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processing software or (1) to calculate the amount of 14 carbamate pesticide residues in the sample.
MA
VcA
Is
.(1)
Where.
X i - Residue of pesticide i in the sample in milligrams per kilogram (mg/kg);
The peak area (or peak height) of carbamate pesticides in sample solution;
Ci - the concentration of pesticide i in standard working fluid, in micrograms per milliliter (g/mL);
V - the final volume of the sample solution in milliliters (mL);
Ais - peak area (or peak height) of pesticide i in standard working fluid;
M - the mass of the sample represented by the final sample, in grams (g).
Note. The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record C 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 the
Record the requirements of D.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of this method is 0.01 mg/kg.
10.2 Recovery rate
The concentration and recovery of this method are given in Appendix E.
Appendix A
(Informative)
Mass spectrometry conditions
Thermo TSQ Quantum Access LC-MS-MS Detection of Carbamate Mass Spectrometry Reference Conditions.
A) ionization mode. electrospray ionization (ESI);
B) electrospray voltage. 4200 V;
C) sheath gas pressure. 0.276 MPa;
D) Auxiliary gas pressure. 0.138 MPa;
E) ion source temperature. 350 C;
F) collision air pressure. 0.20 Pa;
G) Scanning mode. positive ion scanning;
H) Detection method. Multiple reaction monitoring (MRM).
Table A.1 Mass Spectrometric Parameters of 14 Carbamate Pesticides (Multiple Reaction Monitoring Conditions)
Measured object
name
English name Molecular formula CAS number
Mother ion
(M/z)
Ion
(M/z)
Lens fill
Compensation voltage
(V)
collision
energy
(EV)
Reserved
time
(Min)
Oxamyl C7H13N3O3S 023135-22-0 242.1
72.3 * 95 20
2.10
112.2 95 15
Methomyl C5H10N2O2S 16752-77-5 163.1
88.1 * 63 6
2.41
106.1 63 11
Pirimicarb Pirimicarb C11H18N4O2 023103-98-2 239.1
72.4 64 20
3.97
182.2 * 64 15
Aldicarb C7H14N2O2S 000116-06-3 213.1
89.3 * 78 16
5.36
116.3 78 12
Discontinuous Metolcarb C9H11NO2 001129-41-5 166.1
94.3 74 31
5.61
109.3 * 74 8
Bacteria Bendiocarb C11H13NO4 022781-23-3 224.1
109.2 76 17
5.85
167.2 * 76 7
Carbofuran C12H15NO3 001563-66-2 222.1
123.2 77 21
5.85
165.2 * 77 11
Carbaryl C12H11NO2 000063-25-2 202.1
127.2 80 28
6.04
145.2 * 80 10
Furathiocarb C18H26N2O5S 65907-30-4 383.1
195.0 * 77 17
7.94
252.1 77 11
Isoprocarb C11H15NO2 002631-40-5 194.0
95.2 * 80 15
6.34
137.2 80 9
Biethofencarb C14H21NO4 087130-20-9 268.1
124.2 * 72 32
6.59
226.2 72 6
Chinese Journal of Neuromedicine. Chinese Journal of Neuromedicine. Chinese Journal of Neuromedicine
77.3 * 80 34
6.70
152.2 80 6
Propoxur C11H15NO3 114-26-1 210.1
111.2 * 68 14
5.79
168.1 68 5
Methiocarb C11H15NO2S 029973-13-5 226.0
121.2 74 19
6.79
169.1 * 74 10
Note. Add "*" ions for the quantitative ions.
Non-commercial declaration. The parameters listed in Appendix A are performed on a Thermo TSQ Quantum Access LC-Tandem Mass Spectrometer. Listed here
The test instrument model is for reference only and does not involve commercial purposes and encourages standard users to try different manufacturers and models of instruments.
Appendix B
(Informative)
A multi - reaction monitoring (MRM) chromatogram of 14 carbamate pesticides
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 5.61
RT. 1.30 RT. 2.34 RT. 4.42RT. 3.53
NL. 2.31E6
TIC F. c ESI SRM
Ms2 166.100
[94.267-94.269,
109.250-109.252]
MS ICIS
JZBY1-XISHI-2
5. speed off the power of 4 aldicarb
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 5.36
1.28
0.39 0.57
5.164.50 6.003.64 3.99 6.123.56 7.116.332.60 7.523.11 8.632.39 9.85 10.669.529.278.002.24 10.058.13
NL. 7.32E4
TIC F. c ESI SRM
Ms2 213.100
[89.318-89.320,
116.320-116.322]
MS ICIS
JZBY1-XISHI-2
RT. 0.00 - 11.00 SM. 7G
0 1 2 3 4 5 6 7 8 9 10 11
Time (min)
La
Tiv
Ce
RT. 2.10
8.39
5.88
7.173.70 6.79 7.854.79 8.82 10.520.98 3.19 9.601.34 9.992.83 5.550.42 5.22
NL. 5.13E4
TIC F. c ESI SRM ms2
242.100 [72.251-72.253,
112.159-112.161,
121.164-121.166,
MSICIS
JZBY1-XISHI-2
1. kill line Wei 2. Dudu Wei
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 2.41
RT. 3.27 RT. 4.16 RT. 4.74RT. 1.70
6.04
0.79 5.201.220.36 8.956.805.63 8.12 8.50 10.407.28 9.949.41
NL. 4.51E5
TIC F. c ESI SRM
Ms2 163.100
[88.120-88.122,
106.135-106.137]
MS ICIS
JZBY1-XISHI-2
3. pirimicarb
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 3.97
RT. 6.944.962.07 5.723.24 6.102.481.23 1.69 2.93 7.70 8.340.750.42 10.599.378.79 9.81
NL. 2.50E6
TIC F. c ESI SRM
Ms2 239.100
[72.365-72.367,
182.230-182.232]
MS ICIS
JZBY1-XISHI-2
RT. 0.00 - 12.00 SM. 7G
0 1 2 3 4 5 6 7 8 9 10 11 12
Time (min)
La
Tiv
Ce
RT. 5.85
RT. 2.27 RT. 3.13 RT. 3.49RT. 1.31 RT. 4.65 RT. 5.09
NL. 3.53E6
TIC F. c ESI SRM
Ms2 224.100
[109.219-109.221,
167.162-167.164] MS
ICIS JZBY1-XISHI-2
Evil bug
RT. 0.00 - 12.00 SM. 7G
0 1 2 3 4 5 6 7 8 9 10 11 12
Time (min)
La
Tiv
Ce
RT. 5.85
RT. 1.28 RT. 2.14 RT. 7.95RT. 4.55RT. 3.41 RT. 5.11 RT. 8.18
NL. 1.07E7
TIC F. c ESI SRM
Ms2 222.100
[123.164-123.166,
165.155-165.157] MS
ICIS JZBY1-XISHI-2
7. carbofuran 8. Carbaryl
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 6.04
RT. 2.36 RT. 3.40 RT. 5.9 RT. 4.27 RT. 1.78 RT. 5.10 RT. 8.27
NL. 2.76E6
TIC F. c ESI SRM
Ms2 202.100
[127.190-127.192,
145.171-145.173] MS
ICIS JZBY1-XISHI-2
RT. 0.00 - 12.00 SM. 7G
0 1 2 3 4 5 6 7 8 9 10 11 12
Time (min)
La
Tiv
Ce
RT. 6.79
RT. 5.85RT. 3.24RT. 1.16 RT. 2.53 RT. 4.30 RT. 8.03RT. 5.04
NL. 4.15E6
TIC F. c ESI SRM
Ms2 226.000
[121.207-121.209,
169.145-169.147] MS
ICIS JZBY1-XISHI-2
9. Methyl Sulfide
RT. 0.00 - 12.00 SM. 7G
0 1 2 3 4 5 6 7 8 9 10 11 12
Time (min)
La
Tiv
Ce
RT. 5.79
RT. 2.49 RT. 3.23RT. 1.28 RT. 3.69 RT. 4.73 RT. 8.48
NL. 3.69E6
TIC F. c ESI SRM ms2
210.100 [93.226-93.228,
111.208-111.210,
168.148-168.150] MS
ICIS JZBY1-XISHI-2
13. Murdoch
11. Ethylmethrin
RT. 0.00 - 11.00 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 6.59
RT. 1.24 RT. 2.23 RT. 2.86 RT. 4.18 RT. 5.27
NL. 1.38E6
TIC F. c ESI SRM
Ms2 268.100
[124.161-124.163,
226.164-226.166] MS
ICIS JZBY1-XISHI-2
12. Zhong Dingwei
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 6.70
RT. 2.06RT. 1.30 RT. 2.67 RT. 3.51 RT. 4.62 RT. 5.28
NL. 1.61E6
TIC F. c ESI SRM
Ms2 208.100
[77.334-77.336,
152.205-152.207]
MS ICIS
JZBY1-XISHI-2
RT. 0.00 - 11.00 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 7.94
RT. 6.97 RT. 10.57RT. 2.84RT. 0.94 RT. 4.29 RT. 9.28RT. 5.10
NL. 7.95E5
TIC F. c ESI SRM
Ms2 383.100
[195.047-195.049,
252.067-252.069] MS
ICIS JZBY1-XISHI-2
14. Fulian Wei
10. isoprene
RT. 0.00 - 11.01 SM. 7G
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0
Time (min)
La
Tiv
Ce
RT. 6.34
RT. 1.30 RT. 3.55RT. 2.31 RT. 4.32 RT. 5.15
NL. 6.31E6
TIC F. c ESI SRM
Ms2 194.000
[95.194-95.196,
137.172-137.174]
MS ICIS
JZBY1-XISHI-2
Figure B.1 Multi-reaction monitoring (MRM) chromatograms of 14 carbamate pesticides
Appendix C
(Normative appendix)
Laboratory repeatability requirements
Table C.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix D
(Normative appendix)
Inter-laboratory reproducibility requirements
Table D.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
Appendix E
(Informative)
Milk and dairy products in the 14 kinds of carbamate pesticide added recovery range
Table E.1 Recovery range of 14 carbamate pesticides in milk and dairy products (n = 10)
Pesticide Name Sample Name Add Level (mg/kg) Recovery Rate Range (%) RSD%
Kill the line
Pure milk
0.010 81.8 ~ 98.5 6.95
0.050 78.0 ~ 98.4 8.44
0.100 81.8 ~ 99.6 7.27
yogurt
0.010 81.0 ~ 94.5 5.40
0.050 86.4 ~ 102.4 6.84
0.100 90.2 ~ 98.8 3.21
milk powder
0.010 81.0 to 99.0 7.27
0.050 81.0 ~ 96.8 6.53
0.100 81.4 ~ 97.6 5.68
cheese
0.010 80.5 to 93.6 5.60
0.050 83.0 ~ 105.2 7.51
0.100 91.6 ~ 106.3 4.39
Fruit milk
0.010 81.6 ~ 108.0 10.7
0.050 83.2 to 104.8 8.46
0.100 85.5 ~ 108.9 8.57
Mordorius
Pure milk
0.010 80.3 ~ 98.8 6.30
0.050 82.2 ~ 99.2 5.74
0.100 82.1 ~ 101.7 7.13
yogurt
0.010 82.5 ~ 105.1 8.37
0.050 85.2 ~ 102.4 7.50
0.100 81.5 ~ 97.9 5.81
milk powder
0.010 81.6 ~ 95.7 6.62
0.050 80.4 ~ 96.4 6.42
0.100 82.2 ~ 99.7 6.96
cheese
0.010 81.1 ~ 94.8 6.15
0.050 80.4 ~ 96.8 6.07
0.100 82.4 ~ 108.7 9.72
Fruit milk
0.010 81.3 ~ 96.8 5.85
0.050 79.2 ~ 98.0 7.74
0.100 76.5 ~ 92.1 5.99
Pirimicarb
Pure milk
0.010 84.8 ~ 97.8 4.74
0.050 74.2 ~ 88.6 6.41
0.100 80.8 ~ 93.6 5.55
Yogurt 0.010 77.0 ~ 93.5 6.65
0.050 81.0 ~ 102.4 8.66
0.100 92.5 ~ 106.2 5.05
milk powder
0.010 81.0 ~ 97.6 6.38
0.050 82.0 ~ 102.2 7.98
0.100 88.0 to 107.0 5.84
cheese
0.010 82.4 ~ 96.0 6.04
0.050 84.6 ~ 103.2 7.17
0.100 89.3 ~ 108.1 6.12
Fruit milk
0.010 77.6 ~ 86.6 3.62
0.050 82.8 ~ 104.0 7.22
0.100 85.2 ~ 98.7 4.97
Aldicarb
Pure milk
0.010 88.5 to 108.9 6.62
0.050 80.8 ~ 105.6 9.51
0.100 79.2 ~ 99.3 8.27
yogurt
0.010 80.5 to 92.1 5.50
0.050 91.2 ~ 106.4 5.40
0.100 83.1 ~ 108.0 8.64
milk powder
0.010 74.2 ~ 91.0 6.40
0.050 84.0 ~ 97.6 5.66
0.100 84.4 ~ 98.8 5.20
cheese
0.010 78.1 to 98.9 8.91
0.050 80.0 ~ 97.4 7.37
0.100 81.1 ~ 94.7 6.17
Fruit milk
0.010 88.5 to 104.7 4.90
0.050 83.0 ~ 98.6 6.55
0.100 85.0 ~ 98.2 4.59
Speed off
Pure milk
0.010 80.6 ~ 93.5 4.58
0.050 77.8 ~ 93.8 5.63
0.100 82.8 ~ 93.0 3.92
yogurt
0.010 77.3 ~ 95.3 6.56
0.050 87.0 ~ 109.2 7.93
0.100 81.0 ~ 107.9 8.42
milk powder
0.010 80.9 to 94.2 5.59
0.050 83.4 ~ 102.8 6.45
0.100 82.2 ~ 98.1 6.28
cheese
0.010 76.8 ~ 86.1 3.75
0.050 84.2 ~ 106.0 7.83
0.100 78.6 ~ 98.3 7.37
Fruit milk
0.010 82.1 ~ 107.0 7.64
0.050 81.8 ~ 97.2 7.24
0.100 84.1 to 97.2 5.00
Evil worms
Pure milk
0.010 83.2 ~ 94.5 3.96
0.050 81.2 ~ 95.0 5.24
0.100 82.9 ~ 93.3 4.20
yogurt
0.010 80.6 ~ 90.1 4.38
0.050 87.0 ~ 104.2 5.64
0.100 91.2 ~ 102.1 3.56
milk powder
0.010 78.6 ~ 94.0 6.50
0.050 83.6 ~ 96.6 5.48
0.100 81.0 ~ 98.6 7.03
cheese
0.010 76.5 to 88.4 5.38
0.050 82.8 ~ 102.4 7.63
0.100 83.0 ~ 100.1 6.82
Fruit milk
0.010 82.6 ~ 93.6 4.70
0.050 84.2 ~ 98.6 5.99
0.100 81.4 ~ 97.4 6.45
Carbofuran
Pure milk
0.010 84.5 to 98.6 5.43
0.050 83.4 ~ 97.8 4.03
0.100 78.1 ~ 91.9 5.24
yogurt
0.010 80.6 ~ 95.1 5.95
0.050 87.2 ~ 104.8 5.76
0.100 81.0 to 96.4 6.21
milk powder
0.010 83.0 ~ 106.7 8.15
0.050 89.8 ~ 108.6 5.96
0.100 81.4 ~ 95.7 5.85
cheese
0.010 80.1 to 91.4 4.83
0.050 81.8 ~ 102.2 7.67
0.100 80.4 ...
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