Method validation parameters: linearity, linear range, limits of detection (LODs), limits of quantification (LOQs), mean recoveries (%) and relative standard deviations (RSDs%, n = 5) of three different spiked levels (n = 5) studied for intra-day and inter-day, matrix effect (ME%) and process efficiency (PE%) for pharmaceutical residues in seawater
Pharmaceuticals
Linearity (r2)
Linear range(ng L–1)
LOD(ng L–1)
LOQ(ng L–1)
25 ng L–1
100 ng L–1
250 ng L–1
25 ng L–1
100 ng L–1
250 ng L–1
ME%
PE%
Rec (%)
RSDr%
Rec (%)
RSDr%
Rec (%)
RSDr%
Rec (%)
RSDR%
Rec(%)
RSDR%
Rec (%)
RSDR%
Antibiotics
Erythromycin-H2O
0.9977
25–250
6.0
18.5
76.2
1.1
87.6
1.3
87.0
0.9
76.0
1.7
87.4
1.1
86.8
1.1
14.9
100.7
N-Acetyl sulfamethoxazole
0.9989
25–250
1.8
5.3
76.4
0.8
79.2
1.7
75.6
1.3
74.0
1.4
76.8
2.1
78.2
1.9
0.6
79.6
Oxolinic acid
0.9976
25–250
9.8
26.4
85.2
0.9
85.0
1.2
88.6
1.3
78.6
1.5
2.0
86.9
Oxytetracycline
0.9996
12.5–125
5.0
16.7
81.4
1.2
90.0
0.8
86.2
1.3
77.4
1.6
86.0
1.3
82.2
1.5
9.2
98.3
Sulfadiazine
0.9995
25–250
2.5
8.5
86.6
1.1
89.0
1.2
76.6
1.1
82.4
1.2
94.8
2.4
82.4
1.2
–18.8
72.2
Sulfamethazine
0.9996
25–250
2.1
6.0
81.4
1.1
88.8
1.3
86.0
1.4
78.2
2.3
85.4
2.5
82.6
1.4
5.7
93.9
Sulfamethizole
0.9994
25–250
2.5
6.6
61.6
1.3
65.0
1.7
62.4
1.3
62.0
1.8
65.4
2.0
62.8
2.2
5.6
68.6
Sulfamethoxazole
1.0000
25–250
1.1
3.0
92.0
1.7
98.6
1.9
92.6
1.8
98.2
1.9
95.0
2.9
90.8
1.8
–1.8
96.8
Sulfamethoxypyridazine
0.9997
25–250
3.4
10.3
79.4
1.2
87.2
0.8
84.2
1.2
77.4
1.4
85.0
2.9
82.0
2.1
3.1
89.9
Sulfapyridine
0.9995
25–250
3.0
10.0
90.2
1.1
96.8
1.5
96.2
0.9
74.8
1.4
76.6
1.5
76.0
0.9
0.9
97.7
Sulfaquinoxaline
0.9907
25–250
3.3
10.0
71.2
1.0
75.8
1.7
76.2
1.1
70.4
1.3
70.0
2.4
70.4
2.4
6.0
80.3
Sulfathiazole
0.9970
25–250
3.0
9.3
86.8
1.1
86.6
1.5
87.0
1.5
88.4
1.2
88.2
1.9
88.6
1.7
–3.1
84.5
Trimethoprim
0.9975
50–250
5.0
18.0
98.8
0.6
101.2
1.6
98.2
2.2
92.0
1.3
93.0
3.1
95.0
4.2
–0.9
100.2
Stimulant
Caffeine
0.9998
50–250
3.3
10.6
85.2
1.0
105.6
0.5
110.8
0.7
95.0
1.1
115.4
1.3
118.8
1.0
–0.2
105.4
Analgesics
Paracetamol
0.9962
25–250
3.6
9.8
93.4
1.3
110.2
1.0
116.2
0.5
81.8
1.4
98.6
1.5
104.6
1.1
–15.8
92.8
Phenazone
0.9998
25–250
2.5
8.3
81.6
1.1
93.0
0.9
80.8
1.0
85.4
2.1
96.8
1.7
84.4
1.0
–14.4
79.6
Anticonvulsants
Carbamazepine
1.0000
25–250
0.5
1.2
92.6
1.5
92.0
1.3
87.8
0.8
91.8
1.6
91.2
1.3
87.0
1.5
–0.9
91.2
Carbamazepine-10.11-epoxide (M)
0.9949
12.5–125
1.5
4.5
80.0
1.6
83.2
3.9
84.0
1.2
77.4
1.3
80.4
2.2
83.2
4.8
–8.3
76.3
Antidepressants
Citalopram
0.9998
25–250
0.7
2.1
62.6
1.8
81.6
1.0
96.0
1.0
62.0
1.6
88.6
1.5
82.8
1.6
18.1
96.4
Fluoxetine
0.9944
12.5–250
1.4
4.1
84.6
0.6
86.8
1.1
82.0
1.2
85.6
1.1
87.8
2.2
83.0
1.5
14.8
99.6
N-Desmethyl sertraline (M)
0.9942
50–500
3.1
8.5
62.0
1.8
65.4
2.6
68.8
0.9
61.8
3.2
64.0
2.6
64.4
1.8
–0.9
67.8
Norfluoxetine (M)
0.9925
100–500
2.2
6.0
64.6
1.7
69.8
1.2
71.6
1.6
66.6
1.7
64.8
2.0
66.4
1.7
–14.1
60.0
O-Desmethyl venlafaxine
0.9960
25–250
0.8
2.0
77.0
1.4
110.0
1.3
101.0
1.0
74.4
1.9
103.0
1.3
93.8
1.4
8.7
119.6
Sertraline
0.9987
2.5–500
1.3
4.2
85.6
1.4
86.4
1.8
87.8
1.7
82.1
1.1
85.0
2.3
87.8
1.7
0.7
82.7
Venlafaxine
0.9981
25–250
0.3
1.5
68.0
1.2
98.8
1.3
91.0
1.1
69.2
1.2
100.0
1.1
92.4
1.5
4.9
103.7
RSDr repeatability relative standard deviation; RSDR reproducibility relative standard deviation
This research was co-financed by Greece and the European Union (European Social Fund-ESF) through the Operational Programme «Human Resources Development. Education and Lifelong Learning» in the context of the project “Strengthening Human Resources Research Potential via Doctorate Research” (MIS-5000432). Implemented by the State Scholarships Foundation (ΙΚΥ). The authors would like to thank the Unit of Environmental. Organic and Biochemical High-Resolution Analysis-Orbitrap-LC-MS of the University of Ioannina for providing access to the facilities.
All relevant data is contained within the manuscript.
Funding
This research is co-financed by Greece and the European Union (European Social Fund-ESF) through the Operational Programme “Human Resources Development. Education and Lifelong Learning” in the context of the project “Strengthening Human Resources Research Potential via Doctorate Research” [MIS-5000432]. Implemented by the State Scholarships Foundation (ΙΚΥ). The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.
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