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GB 23200.90-2016Food safety national standard -- Determination of various carbamate pesticide residues in milk and dairy products by liquid chromatography-mass spectrometry (English PDF)

乳及乳制品中多种氨基甲酸酯类农药残留量的测定液相色谱-质谱法

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Issued by

National Health and Family Planning Commission of the People 's Republic of China

Level / Type

National · Mandatory

Issue date

December 18, 2016

Implementation date

June 18, 2017

Scope

GB 23200.90-2016 is the English-translated version of 乳及乳制品中多种氨基甲酸酯类农药残留量的测定液相色谱-质谱法.

GB 23200.90-2016 — 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.

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Document preview — GB 23200.90-2016

National Standard of the People's Republic of China

Classification: G 25
Replacing: SN/T 3156-2012

Issued by: National Health and Family Planning Commission of the People 's Republic of China

Foreword
1 Scope
2 Normative reference documents
3 Principle
4 Reagents and materials
4.1 Reagents
4.2 Standards
4.3 Standard solution preparation
4.4 Materials
5 Instruments and equipment
6 Sample preservation
7 Analysis steps
7.1 Extraction
7.2 Purification
7.3 Determination
7.4 Blank test
8 Results are calculated and expressed
9 Precision
10.1 Quantitation limits
10.2 Recovery rate
13 Murdoch
14 Fulian Wei

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.

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

(ML/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.

xxx=

VcA

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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