Sensing Application — High efficient solid-phase microextraction based on a covalent organic framework for determination of trifluralin and chlorpyrifos in water and food samples by GC-CD-IMS

5 measurement groups · 45 results

Reported values remain attached to the sample, method, conditions, extraction quality and source location that produced them.

SPME-GC-CD-IMS method validation in spiked distilled water

COF-coated SPME fibre · Thin Film

Analytical figures of merit for trifluralin and chlorpyrifos under optimum extraction conditions.

Geometry: COF-coated SPME fibre coupled to GC with corona discharge ion mobility spectrometer detector
Context: composite SPME fibre using pristine COF sorbent
Measurement source: p005 · 3.3. Method validation · Table 1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Chlorpyrifos extraction enrichment factorMarked as a best value within this paper	2123	—	—	Text Exact Reported	p005 · 3.3. Method validation
Chlorpyrifos linear dynamic range	0.50-25 ug/L	—	range	Table Range	p005 · 3.3. Method validation · Table 1
Chlorpyrifos LODMarked as a best value within this paper	0.15 ug/L	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Chlorpyrifos LOQ	0.50 ug/L	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Chlorpyrifos determination coefficient	0.9987	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Fibre-to-fibre reproducibility RSD	9%	—	<=	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Maximum inter-day repeatability RSD in Table 1	11%	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Maximum intra-day repeatability RSD in Table 1	6%	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Trifluralin extraction enrichment factor	1950	—	—	Text Exact Reported	p005 · 3.3. Method validation
Trifluralin linear dynamic range	0.45-20 ug/L	—	range	Table Range	p005 · 3.3. Method validation · Table 1
Trifluralin LODMarked as a best value within this paper	0.13 ug/L	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Trifluralin LOQ	0.45 ug/L	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1
Trifluralin determination coefficient	0.9965	—	—	Table Exact Reported	p005 · 3.3. Method validation · Table 1

GC-CD-IMS operating-condition table for analyte detection

COF-coated SPME fibre · Thin Film

Typical CD-IMS operating conditions reported in SI Table S1: needle and target electrode voltages, drift field, gas flows, drift tube temperature, shutter grid pulse, IMS averaging, and mobility-spectrum points.

Temperature: 473.15
Atmosphere: N2 drift gas and make-up gas
Geometry: Corona discharge-ion mobility spectrometer coupled to GC; Table S1 operating settings
Context: COF-coated SPME fibre analytical method context
Measurement source: p002 · Table S1 · Table S1

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
CD-IMS drift field	500 V/cm	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS drift gas flow	700 mL/min	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS drift tube temperature	200 C	473.15 K	—	SI Table Exact Reported	p002 · Table S1 · Table S1
Number of IMS averages	25	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS make-up gas flow	20 mL/min	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
Number of points per ion mobility spectrum	500	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS needle voltage	10.5 kV	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS shutter grid pulse	0.3 ms	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1
CD-IMS target electrode voltage	7.5 kv	—	—	SI Table Exact Reported	p002 · Table S1 · Table S1

CD-IMS and GC-CD-IMS separation of trifluralin and chlorpyrifos

COF-coated SPME fibre · Thin Film

Individual solutions and a mixture of trifluralin and chlorpyrifos were analysed to show overlapping IMS spectra and separation by GC-CD-IMS.

Geometry: Thermal desorption injection port at 220 deg C for Fig. 2a; GC-CD-IMS chromatogram in 10.50-12.00 ms drift-time window for Fig. 2b
Context: application context for composite SPME fibre and GC-CD-IMS detection
Measurement source: p005 · 3.3. Method validation · Fig. 2

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Approximate chlorpyrifos retention time in GC-CD-IMS chromatogram	about 6.8 min	—	about	Figure Axis Approximate	p005 · Figure 2 · Fig. 2b
Approximate trifluralin retention time in GC-CD-IMS chromatogram	about 4.8 min	—	about	Figure Axis Approximate	p005 · Figure 2 · Fig. 2b

SPME-GC-CD-IMS real-sample pesticide analysis

COF-coated SPME fibre · Thin Film

Agricultural wastewater, carrot, cucumber, and grape samples analysed using multiple standard addition; units are ug/L for wastewater and ug/kg for food samples.

Geometry: COF-coated SPME fibre applied to real samples and analysed by GC-CD-IMS
Context: composite SPME fibre using pristine COF sorbent
Measurement source: p006 · 3.4. Analysis of the real samples · Table 2; Fig. 3

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Minimum carrot recovery	87%	—	—	Table Exact Reported	p006 · 3.4. Analysis of real samples · Table 2
Cucumber chlorpyrifos found in unspiked sample	5.6 ug/kg (RSD 6%)	—	RSD 6%	Table Exact Reported	p006 · 3.4. Analysis of the real samples · Table 2
Maximum cucumber recovery	108%	—	—	Table Exact Reported	p006 · 3.4. Analysis of real samples · Table 2
Cucumber trifluralin found in unspiked sample	2.4 ug/kg (RSD 5%)	—	RSD 5%	Table Exact Reported	p006 · 3.4. Analysis of the real samples · Table 2
Grape chlorpyrifos found in unspiked sample	1.5 ug/kg (RSD 6%)	—	RSD 6%	Table Exact Reported	p006 · 3.4. Analysis of the real samples · Table 2
Maximum grape recovery	110%	—	—	Table Exact Reported	p006 · 3.4. Analysis of real samples · Table 2
Grape trifluralin found in unspiked sample	5.9 ug/kg (RSD 3%)	—	RSD 3%	Table Exact Reported	p006 · 3.4. Analysis of the real samples · Table 2
Paired t-test value for chlorpyrifos vs EPA standard methods	3.5	—	—	Text Exact Reported	p006 · 3.4. Analysis of the real samples
Paired t-test value for trifluralin vs EPA standard methods	1.4	—	—	Text Exact Reported	p006 · 3.4. Analysis of the real samples
Relative recovery range across spiked real samplesMarked as a best value within this paper	87% to 110%	—	range	Text Range	p006 · 3.4. Analysis of the real samples · Table 2
Agricultural wastewater chlorpyrifos found in unspiked sample	1.2 ug/L (RSD 7%)	—	RSD 7%	Table Exact Reported	p006 · 3.4. Analysis of the real samples · Table 2
Agricultural wastewater trifluralin recovery at 1.0 ug/L added	90%	—	—	Table Exact Reported	p006 · 3.4. Analysis of real samples · Table 2
Agricultural wastewater chlorpyrifos recovery at 5.0 ug/L added	104%	—	—	Table Exact Reported	p006 · 3.4. Analysis of real samples · Table 2

SPME extraction optimisation for trifluralin and chlorpyrifos

COF-coated SPME fibre · Thin Film

10 mL aqueous sample solution; variables included stirring rate, ionic strength, extraction temperature, extraction time, pH, desorption temperature, and desorption time.

Geometry: COF-coated SPME fibre immersed in analyte solution and thermally desorbed in GC injector
Context: composite SPME fibre using pristine COF as sorbent layer
Measurement source: p004-p005 · 3.2. Optimization of the SPME method · Fig. S9-S14

Property	Reported value	Normalised value	Uncertainty	Origin and quality	Source
Fibre durabilityMarked as a best value within this paper	over 100 cycles without significant efficiency decrease	—	>	Text Approximate	p004 · 3.2.7. Fiber durability
Optimised desorption/injector temperatureMarked as a best value within this paper	230 C	—	—	Text Exact Reported	p004 · 3.2.6. Desorption temperature and time · Fig. S14
Optimised desorption timeMarked as a best value within this paper	3 min	—	—	Text Exact Reported	p004 · 3.2.6. Desorption temperature and time · Fig. S14
Optimised extraction temperatureMarked as a best value within this paper	35 C	—	—	Text Exact Reported	p004 · 3.2.3. Extraction temperature · Fig. S11
Optimised extraction timeMarked as a best value within this paper	30 min	—	—	Text Exact Reported	p004 · 3.2.4. Extraction time · Fig. S12
Ionic strength effect	0 to 10 w/v% NaCl tested; extraction decreased with increasing salt concentration	—	—	Text Qualitative	p004 · 3.2.2. Ionic strength · Fig. S10
Optimised extraction pHMarked as a best value within this paper	pH = 4	—	—	Text Exact Reported	p004 · 3.2.5. pH · Fig. S13
Optimised stirring rateMarked as a best value within this paper	800 rpm	—	—	Text Exact Reported	p004 · 3.2.1. Stirring rate · Fig. S9