Apparent recovery (%) |
n=18*/21** |
1.00*/0.50** |
125.8 |
85.4 |
64.5 |
98.8 |
2.00/1.00 |
104.7 |
101.7 |
65.9 |
94.0 |
3.00/1.50 |
88.4 |
90.7 |
66.8 |
88.7 |
n = 18*/6** |
4.00/2.00 |
87.4 |
94.3 |
98.8 |
103.2 |
10.00/5.00 |
81.1 |
88.0 |
96.4 |
97.1 |
n= 6** |
CCα** |
NE |
NE |
91.9 |
114.6 |
Repeatability (RSD, %) |
n=18*/21** |
1.00*/0.50** |
22.4 |
24.0 |
11.2 |
4.4 |
2.00/1.00 |
22.7 |
19.2 |
6.8 |
6.1 |
3.00/1.50 |
12.9 |
17.5 |
7.3 |
4.4 |
4.00/2.00 |
20.9 |
11.9 |
6.7 |
13.4 |
n = 18*/6** |
10.00/5.00 |
27.7 |
13.6 |
7.9 |
12.1 |
n = 6** |
CCα** |
NE |
NE |
15.3 |
10.7 |
Within-lab reproducibility (RSD, %) |
n=18*/21** |
2.00*/0.50** |
27.2 |
22.9 |
23.8 |
10.5 |
3.00/1.00 |
22.0 |
17.6 |
15.2 |
17.7 |
4.00/1.50 |
30.2 |
12.3 |
10.9 |
10.9 |
Decision limit (CCα, μg L−1) |
0.44 |
0.25 |
0.14 |
0.08 |
Detection capability (CCβ, μg L−1) |
0.75 |
0.42 |
0.24 |
0.13 |
Measurement uncertainty at validation level of *2 μg L−1/**1 μg L−1 (U, k = 2, μg L−1/ %) |
0.37/18.5 |
0.31/15.5 |
0.20/20.0 |
0.34/34.0 |
Matrix effect (ME, %) |
NE |
NE |
7.0 |
10.0 |
Standard calibration curve |
Slope ± sb |
0.2119 ± 0.0843 |
0.1058 ± 0.2351 |
0.2112 ± 0.2456 |
0.1443 ± 0.0845 |
y-Intercept ± sa |
0.0812 ± 0.0838 |
−0.0027 ± 0.0737 |
0.0570 ± 0.0424 |
0.0125 ± 0.0096 |
Correlation coefficient |
0.9945 |
0.9985 |
0.9866 |
0.9970 |
Standard error |
0.0662 |
0.0127 |
0.0884 |
0.0285 |
Matrix matched calibration curve |
Slope ± sb |
0.1781 ± 0.1220 |
0.1228 ± 0.0223 |
0.2516 ± 0.1005 |
0.1564 ± 0.0554 |
y-Intercept ± sa |
0.1656 ± 0.1199 |
−0.0102 ± 0.0088 |
−0.0322 ± 0.0291 |
−0.0060 ± 0.0103 |
Correlation coefficient |
0.9983 |
0.9995 |
0.0291 |
0.9988 |
Standard error |
0.0426 |
0.0156 |
0.0582 |
0.0148 |
Additional series of validation** |
Compound |
Number of samples |
Spiking level (μg L−1) |
STAN |
16β-OH-STAN |
Apparent recovery (%)// |
n = 7 |
0.25 |
89.4//3.1 |
102.7//6.7 |
0.50 |
70.2//4.4 |
108.3//1.8 |
0.75 |
79.8//10.2 |
101.7//4.5 |
Repeatability (RSD, %) |
n = 4 |
1.00 |
80.5//5.5 |
100.2//4.7 |
2.00 |
86.8//15.9 |
96.5//3.1 |
5.00 |
81.4//9.0 |
94.0//2.9 |
n = 10 |
CCα |
105.0//4.9 |
101.3//20.0 |
Decision limit (CCα, μg L−1) |
0.27 |
0.28 |
Standard curve: Equation/Correlation coefficient |
y = 0.6440x-0.0664/0.9998 |
y = 0.1570x-0.0168/0.9971 |
Matrix matched calibration curve: Equation/Correlation coefficient |
y = 0.5230x-0.0670/0.9997 |
y = 0.1453x-0.0033/1.0000 |