In Situ Real-Time Tracing of Organophosphorus Pesticides in Apples by Solid-Phase Microextraction with Developed Sampling-Rate Calibration
Abstract
:1. Introduction
2. Results and Discussion
2.1. Strategies to Ensure the Lifetime of the Fiber in Apple Matrix
2.2. Stability of OPPs in Apple Matrix and Analytical Performance of the Fiber
2.3. Preparation of Positive Samples for In Situ Analysis
2.4. and Its Applicability
2.5. Evaluation of In Situ SPME/GC Method
2.6. In Situ Tracing OPPs in Apples
3. Materials and Methods
3.1. Chemical Reagents, Materials, and Samples
3.2. Instruments and Chromatographic Conditions
3.3. Preparation of SPME Fibers, SPME Procedure, LLE Procedure
3.4. In Situ SPME
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are not available from the authors. |
Analyte | Linear Range (ng/g) | R2 | LOD a (ng/g) | LOQ b (ng/g) | RSD c (%) | Spiking Level (ng/g) | Recovery (%) |
---|---|---|---|---|---|---|---|
Diazinon | 1.25–25 | 0.9996 | 0.02 | 0.07 | 8.11 | 2.5 | 89.90 ± 4.89 |
12.5 | 86.31 ± 9.21 | ||||||
25 | 87.56 ± 11.96 | ||||||
Chlorpyrifos | 1.25–250 | 0.9991 | 0.10 | 0.33 | 4.08 | 12.5 | 74.82 ± 6.64 |
25 | 90.02 ± 8.91 | ||||||
125 | 98.50 ± 8.84 |
Analyte | Sampling Time (min) | Concentration (µg/g) | RSD% |
---|---|---|---|
Diazinon | 3 10 20 | 1.61 ± 0.04 1.70 ± 0.11 1.64 ± 0.06 | 4.92 |
Chlorpyrifos | 3 10 20 | 2.10 ± 0.01 2.10 ± 0.01 2.10 ± 0.01 | 0.30 |
Analyte | t (min) | Concentration (µg/g) | RSD% | |
---|---|---|---|---|
In situ SPME/GC | LLE/GC | |||
Diazinon | 15 | 1.62 ± 0.28 a | 2.62 ± 0.31 | 29.21 |
18 | 2.02 ± 0.48 b | 2.07 ± 0.12 | 1.7 | |
20 | 1.26 ± 0.16 c | 1.24 ± 0.10 | 0.95 | |
22 | 1.19 ± 0.16 c | 1.36 ± 0.03 | 9.25 | |
25 | 1.12 ± 0.16 c | 1.54 ± 0.01 | 22.24 | |
30 | 1.02 ± 0.39 c | 1.73 ± 0.12 | 38.54 | |
40 | 0.90 ± 0.30 c | 1.64 ± 0.03 | 39.65 | |
Chlorpyrifos | 15 | 4.20 ± 0.31 a | 5.09 ± 0.56 | 12.38 |
18 | 5.02 ± 0.25 b | 5.06 ± 0.39 | 0.59 | |
20 | 3.62 ± 0.12 c | 3.25 ± 0.02 | 8.87 | |
22 | 3.42 ± 0.09 c | 3.58 ± 0.09 | 3.39 | |
25 | 3.12 ± 0.11 c | 3.82 ± 0.10 | 14.4 | |
30 | 2.51 ± 0.14 d | 3.92 ± 0.22 | 30.26 | |
40 | 1.95 ± 0.19 e | 4.05 ± 0.11 | 40.75 |
Analyte | LOD (ng/g) | LOQ (ng/g) | RSD% |
---|---|---|---|
Diazinon | 0.18 | 0.60 | 2.28 |
Chlorpyrifos | 0.20 | 0.67 | 0.28 |
Analyte | Soaking Concentration (µg/mL) | Concentration (µg/g) | RSD% | |
---|---|---|---|---|
In Situ SPME/GC | LLE/GC | |||
Diazinon | 20 | 1.32 ± 0.02 | 1.13 ± 0.01 | 7.9 |
40 | 1.58 ± 0.12 | 1.75 ± 0.01 | 7.75 | |
60 | 1.64 ± 0.02 | 1.84 ± 0.09 | 6.04 | |
Chlorpyrifos | 20 | 2.73 ± 0.01 | 2.22 ± 0.02 | 9.79 |
40 | 2.80 ± 0.02 | 2.88 ± 0.32 | 6.22 | |
60 | 2.62 ± 0.02 | 2.85 ± 0.09 | 4.91 |
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Zhang, X.-F.; Zhao, L.-L.; Huang, M.-Q.; Li, X.-J.; Pan, S.-Y. In Situ Real-Time Tracing of Organophosphorus Pesticides in Apples by Solid-Phase Microextraction with Developed Sampling-Rate Calibration. Molecules 2019, 24, 4444. https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24244444
Zhang X-F, Zhao L-L, Huang M-Q, Li X-J, Pan S-Y. In Situ Real-Time Tracing of Organophosphorus Pesticides in Apples by Solid-Phase Microextraction with Developed Sampling-Rate Calibration. Molecules. 2019; 24(24):4444. https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24244444
Chicago/Turabian StyleZhang, Xiao-Fan, Li-Li Zhao, Ming-Quan Huang, Xiu-Juan Li, and Si-Yi Pan. 2019. "In Situ Real-Time Tracing of Organophosphorus Pesticides in Apples by Solid-Phase Microextraction with Developed Sampling-Rate Calibration" Molecules 24, no. 24: 4444. https://0-doi-org.brum.beds.ac.uk/10.3390/molecules24244444