Page 77 - Application Notebook - Solution for Food Safety

Application No.C140
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Table 2 Analytical Conditions
System : Nexera X2 System : LCMS-8060
Column : ACE SuperC18 (100 mm L. × 2.1 mm I.D., 2 μm) Ionization : Heated ESI
Column Temperature : 30 °C Probe Voltage : +1 kV (positive ionization) /
Mobile Phases : A: Water = 0.05 % ammonia -1.5 kV (negative ionization)
B: Methanol + 0.05 % ammonia Temperature : Interface: 400 °C
Flowrate : 600 μL/min Desolvation Line: 200 °C
Gradient : 5 %B to 100 %B in 3 min Heater Block: 400 °C
100 %B to 5 %B in 0.1 min Gas Flow : Nebulizing Gas: 3 L/min
Total Run Time : 4 min Heating Gas: 10 L/min
Injection Volume : 2 μL (POISe mode with 10 μL of water) Drying Gas: 5 L/min

Table 3 MS/MS Acquisition Parameters
MRM Transitions Name Polarity MRM Quan MRM Qual ISTD
Acetamiprid + 223.1 > 126.0 223.1 > 56.1 2
Acetamiprid-N-desmethyl + 209.1 > 126.0 211.1 > 128.0 2
Clothianidin + 250.1 > 169.1 250.1 > 132.0 3
Dinotefuran + 203.0 > 114.0 203.0 > 87.0 1
Fipronil - 435.0 > 330.0 435.0 > 250.0 3
Fipronil sulfone - 451.0 > 415.0 451.0 > 282.0 3
Imidacloprid + 256.1 > 175.1 258.1 > 211.1 2
Nitenpyram + 271.0 > 126.0 271.0 > 225.0 3
Thiacloprid + 253.1 > 126 253.1 > 90.1 1
Thiamethoxam + 292.1 > 211.1 292.1 > 181.1 1

Thiamethoxam-D3 + 295.1 > 214.05 --- 1
Imidacloprid-D4 + 260.1 > 179.1 --- 2
Clothianidin-D3 + 253.1 > 132.05 --- 3

Dwell Time : 3 to 34 msec depending upon the number of concomitant transitions to ensure to
have at least 30 points per peak (max total loop time 140 msec).
Pause Time : 1 msec
Quadrupole Resolution : Q1: Unit Q3: Unit

Q Calibration Area Ratio 37.5 y = 0.0x 2 + 0.008386x + 0.040184 n = 1
R 2 = 0.9988971 R = 0.9994484
Calibration curves were prepared in acetonitrile to 35.0 Curve Fit: Quadratic
32.5 Weighting: 1/x
obtain final concentrations ranging from 0.5 pg/mL 30.0 Zero: Default (Not Forced)
(1 fg on column) to 5 ng/mL. These concentrations 27.5 Mean RF: 6.529647
25.0 SD RF: 12.56448
corresponds to 1 ng/kg and 10 μg/kg in honey, 22.5 %RSD: 192.4221
respectively. 20.0
For each compound, the lower limit of quantification 17.5
15.0
was selected to give an accuracy between 80-120 % 12.5
(see table 4). 10.0
A typical calibration curve is shown in Fig. 2. 7.5
5.0
2.5
0.0
Table 4 Limits of Quantification in Honey 0 250 500 750 1000 1250 1500 1750 2000 2250 2500 2750 3000 3250 3500 3750 4000 4250 4500 4750 5000
Conc.Ratio
LOQ LOQ Standard (μg/kg) Accuracy (%)
Compound Compound
(μg/kg) (μg/kg) 0.005 106
Acetamiprid 0.005 Fipronil sulfone 0.001
0.010 97.2
Acetamiprid-N-desmethyl 0.005 Imidacloprid 0.020
0.020 95.6
Chlothianidin 0.020 Nitenpyram 0.020
0.100 107
Dinotefuran 0.010 Thiacloprid 0.005
Fipronil 0.001 Thiamethoxam 0.005 0.200 98.4
0.500 91.5
1.000 104
5.000 99.9
10.000 100
Fig. 2 Calibration Curve of Acetamiprid