Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil
Abstract
:1. Introduction
2. Results and Discussion
2.1. Determination of the Conditions for the HPLC Detection Method
2.2. Single Factor Tests of Ultrasonic Extraction Pretreatment
2.2.1. Volumes of Extraction Solution
2.2.2. pH Values of Extraction Solution
2.2.3. Ultrasonication Time
2.2.4. Ultrasonication Temperature
2.2.5. Total Cycles of Extraction
2.3. RSM Optimization
2.4. Method Validation for Real Samples
2.5. Comparison with Other Existing Methods
3. Materials and Methods
3.1. Materials and Reagents
3.2. Sample Processing
3.3. Detection Conditions with HPLC
3.4. Extraction Method
3.5. Single-Factor Experiments
3.6. Response Surface Optimization (RSM)
3.7. Method Validation
4. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are not available from the authors. |
Compound | Linear Regression Equation | R2 | LOD (μg/kg) | LOQ (μg/kg) |
---|---|---|---|---|
SMZ | Y = 33.696X + 2115.651 | 0.99998 | 0.3 | 1 |
E2 | Y = 4.367X + 60.425 | 0.99991 | 10 | 30 |
X1 | X2 | X3 | Y | |
---|---|---|---|---|
Ultrasonication Time (min) | pH Values | Volume (mL) | Recovery (%) | |
1 | 20.00 (−1) | 4.00 (0) | 50.00 (+1) | 69.12 |
2 | 30.00 (0) | 4.00 (0) | 40.00 (0) | 81.70 |
3 | 30.00 (0) | 3.00 (−1) | 30.00 (−1) | 65.97 |
4 | 30.00 (0) | 5.00 (+1) | 30.00 (−1) | 69.64 |
5 | 30.00 (0) | 5.00 (+1) | 50.00 (+1) | 73.13 |
6 | 40.00 (+1) | 3.00 (−1) | 40.00 (0) | 68.91 |
7 | 20.00 (−1) | 4.00 (0) | 30.00 (−1) | 74.78 |
8 | 20.00 (−1) | 5.00 (+1) | 40.00 (0) | 70.75 |
9 | 40.00 (+1) | 5.00 (+1) | 40.00 (0) | 76.72 |
10 | 40.00 (+1) | 4.00 (0) | 50.00 (+1) | 75.57 |
11 | 30.00 (0) | 4.00 (0) | 40.00 (0) | 80.59 |
12 | 40.00 (+1) | 4.00 (0) | 30.00 (−1) | 75.36 |
13 | 30.00 (0) | 3.00 (−1) | 50.00 (+1) | 62.71 |
14 | 20.00 (−1) | 3.00 (−1) | 40.00 (0) | 71.88 |
15 | 30.00 (0) | 4.00 (0) | 40.00 (0) | 81.30 |
Source | Sum of Squares | Df a | Mean Square | F-value b | P value c |
---|---|---|---|---|---|
Model | 421.87 | 9 | 46.87 | 17.29 | 0.0029 |
X1, time (min) | 12.58 | 1 | 12.58 | 4.64 | 0.0839 |
X2, pH | 53.92 | 1 | 53.92 | 19.89 | 0.0066 |
X3, volume (mL) | 3.41 | 1 | 3.41 | 1.26 | 0.3133 |
X1X2 | 19.98 | 1 | 19.98 | 7.37 | 0.0421 |
X1X3 | 8.61 | 1 | 8.61 | 3.18 | 0.1348 |
X2X3 | 11.39 | 1 | 11.39 | 4.20 | 0.0957 |
X12 | 9.97 | 1 | 9.97 | 3.68 | 0.1133 |
X22 | 207.05 | 1 | 207.05 | 76.35 | 0.0003 |
X32 | 126.18 | 1 | 126.18 | 46.53 | 0.0010 |
Residual | 13.56 | 5 | 2.71 | ||
Lack of fit | 12.93 | 3 | 4.31 | 13.63 | 0.0691 |
Pure error | 0.63 | 2 | 0.32 | ||
R2 | 0.9689 | ||||
Adj R2 | 0.9128 |
Added (mg/kg) | Soil Samples a | SMZ Recovery (%) | E2 Recovery (%) | Average Recovery (%) | Integral Average Recovery (%) | RSD b (%) |
---|---|---|---|---|---|---|
20 | S1 | 84.85 ± 0.81 | 81.26 ± 0.83 | 83.06 ± 0.68 | 81.78 ± 1.62 | 1.62 |
S2 | 82.32 ± 2.63 | 76.66 ± 0.97 | 79.49 ± 0.85 | |||
S3 | 87.51 ± 1.66 | 78.07 ± 2.90 | 82.79 ± 1.81 | |||
40 | S1 | 78.79 ± 2.96 | 86.06 ± 2.01 | 82.42 ± 4.81 | 82.02 ± 0.25 | 0.24 |
S2 | 74.67 ± 1.29 | 89.32 ± 1.81 | 81.99 ± 1.51 | |||
S3 | 76.54 ± 1.90 | 87.14 ± 0.46 | 81.84 ± 0.74 | |||
60 | S1 | 80.66 ± 2.35 | 88.27 ± 1.53 | 86.47 ± 0.57 | 85.05 ± 1.00 | 3.55 |
S2 | 81.72 ± 1.74 | 86.86 ± 0.92 | 84.29 ± 0.86 | |||
S3 | 82.44 ± 1.31 | 86.35 ± 1.55 | 84.40 ± 0.36 |
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Song, R.; Chen, Q.; Yan, L.; Rao, P.; Sun, P.; Wang, L.; Shen, G. Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil. Molecules 2020, 25, 1415. https://doi.org/10.3390/molecules25061415
Song R, Chen Q, Yan L, Rao P, Sun P, Wang L, Shen G. Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil. Molecules. 2020; 25(6):1415. https://doi.org/10.3390/molecules25061415
Chicago/Turabian StyleSong, Rui, Qincheng Chen, Lili Yan, Pinhua Rao, Peng Sun, Lumei Wang, and Guoqing Shen. 2020. "Response Surface Optimization of an Extraction Method for the Simultaneous Detection of Sulfamethoxazole and 17β-Estradiol in Soil" Molecules 25, no. 6: 1415. https://doi.org/10.3390/molecules25061415