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. 2020 May 19;8:423. doi: 10.3389/fchem.2020.00423

Table 2.

Performance characteristics of the method as obtained during in-house validation on the QTrap6500+ instrument including concentration range of matrix matched standard calibration, regression coefficient (R2), spiking levels, recoveries of the extraction step (RE), intermediate precision (RSDR), repeatability (RSDr), signal suppression/enhancement (SSE), limits of detection (LOD) and limits of quantification (LOQ).

Analyte Regression coefficients Spiking levela RE ± RSDR low level RE ± RSDR intermediate level RE ± RSDR high level RSDrb SSEc LOD LOQ
R2 [ng/L] [%] [%] [%] [%] [ng/L] [ng/L]
Aflatoxicol 0.9997 50/240/1200 91 ± 3 101 ± 4 96 ± 4 3/4/3 60 30 60
Aflatoxin B1 0.9995 10/48/240 96 ± 2 89 ± 4 84 ± 4 2/6/2 62 2.5 5.0
Aflatoxin B2 0.9997 20/48/240 100 ± 5 87 ± 6 84 ± 5 6/8/4 59 1.0 2.0
Aflatoxin G1 0.9997 30/48/240 99 ± 1 91 ± 7 88 ± 3 2/10/1 70 3.5 7.0
Aflatoxin G2 0.9996 30/48/240 100 ± 8 91 ± 8 90 ± 4 9/10/2 76 4.0 8.0
Aflatoxin M1 0.9997 10/48/240 109 ± 4 84 ± 5 92 ± 3 5/5/3 89 2.0 4.0
Aflatoxin M2 0.9994 48/100/240 87 ± 13 93 ± 8 88 ± 6 20/13/4 88 14 28
Aflatoxin P1 0.9995 48/80/240 91 ± 7 95 ± 6 89 ± 4 6/7/3 49 9.0 18
Aflatoxin Q1 0.9997 10/48/240 89 ± 8 91 ± 11 93 ± 4 6/13/2 75 13 26
Aflatoxin B1-N7-guanine 0.9997 20/240/1200 39 ± 19 22 ± 19 25 ± 25 26/20/38 90 4.0 8.0
Alternariold 0.9996 50/96/480 - - 6 ± 27 -/-/36 44 4.0 8.0
Alternariol monomethyl ethere 0.9998 10/96/480 86 ± 5 89 ± 4 86 ± 4 5/3/3 51 0.5 1.0
Beauvericine 0.9993 6/10/48 85 ± 9 86 ± 6 87 ± 3 10/6/2 76 0.1 0.2
Citrinin 0.9998 6/48/240 118 ± 18 93 ± 4 88 ± 3 15/9/2 115 3.0 6.0
Deoxynivalenold 0.9997 720/1000/3600 - - - -/-/- 89 106 212
Dihydrocitrinone 0.9994 96/200/480 55 ± 7 41 ± 9 46 ± 15 4/14/17 114 14 28
Enniatin A 0.9997 6/10/48 99 ± 5 103 ± 6 99 ± 6 5/7/7 71 0.5 1.0
Enniatin A1 0.9994 6/10/48 98 ± 5 102 ± 8 97 ± 5 4/3/3 86 0.9 1.8
Enniatin Be 0.9997 6/10/48 85 ± 6 99 ± 11 87 ± 7 9/14/9 61 0.7 1.4
Enniatin B1e 0.9995 6/10/48 95 ± 6 100 ± 7 95 ± 5 4/7/4 71 0.5 1.0
HT-2 toxin 0.9966 720/2830/3600 84 ± 12 81 ± 9 98 ± 6 9/9/7 74 300 600
Nivalenold 0.9998 800/1280/6400 - - - -/-/- 91 70 140
Ochratoxin Ae 0.9997 30/96/480 96 ± 3 109 ± 5 104 ± 5 4/3/3 80 0.8 1.5
Ochratoxin B 0.9997 20/96/480 97 ± 3 108 ± 5 105 ± 5 3/4/2 88 2.5 5.0
Ochratoxin α 0.9984 160/300/800 83 ± 18 75 ± 17 84 ± 4 24/23/8 93 24 48
Sterigmatocystin 0.9997 15/24/120 90 ± 2 86 ± 4 84 ± 4 2/3/2 34 0.5 1.0
T-2 toxin 0.9998 96/100/480 106 ± 5 95 ± 2 99 ± 5 6/2/4 55 11 22
Tentoxin 0.9995 96/200/480 101 ± 4 93 ± 3 101 ± 6 5/3/4 76 23 46
Zearalanone 0.9995 96/480/700 92 ± 4 89 ± 4 96 ± 2 3/3/1 50 60 120
α-Zearalanol 0.9996 128/640/800 103 ± 3 98 ± 5 97 ± 2 3/5/2 39 73 146
β-Zearalanol 0.9993 128/640/1200 98 ± 4 93 ± 5 95 ± 1 5/4/1 60 75 150
Zearalenonee 0.9997 96/100/480 103 ± 5 95 ± 3 98 ± 4 4/3/2 53 16 32
α-Zearalenol 0.9995 100/128/640 90 ± 5 103 ± 4 100 ± 5 5/5/4 48 44 87
β-Zearalenol 0.9997 100/128/640 92 ± 5 97 ± 6 93 ± 3 5/5/3 46 54 108
a

Spiking levels reported in the following order: low level/ intermediate level/ high level.

b

RSDr values reported in the following order: low level/ intermediate level/ high level.

c

SSE calculated as the slope of calibration in matrix divided by the slope of calibration in solution expressed in percent.

d

AOH, DON and NIV could not be recovered following our extraction procedure with the exception of AOH at the highest spiked level. Therefore, none of these toxins were successfully validated.

e

Non-spiked pooled matrix sample was contaminated. Therefore, validation results reported were evaluated by standard addition.