Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (4): 323-332.DOI: 10.3724/SP.J.1123.2021.07014
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LING Huijuan1, WU Gege1,*(), LI Shuang1, ZHOU Qian2, LI Chunxin2, MA Jiping1,*()
Received:
2021-07-26
Online:
2022-04-08
Published:
2022-04-01
Contact:
WU Gege, MA Jiping
Supported by:
CLC Number:
LING Huijuan, WU Gege, LI Shuang, ZHOU Qian, LI Chunxin, MA Jiping. Determination of five nonsteroidal anti-inflammatory drugs in water by dispersive solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry based on metal-organic framework composite aerogel[J]. Chinese Journal of Chromatography, 2022, 40(4): 323-332.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.07014
Analyte | tR/min | Precursor ion (m/z) | Product ions (m/z) | Declustering potentials/V | Collision energies/eV |
---|---|---|---|---|---|
Ketoprofen (KPF) | 6.44 | 253.0 | 209.0*, 197.0 | -36, -36 | -8, -19 |
Naproxen (NPX) | 6.73 | 229.3 | 169.8*, 184.8 | -38, -38 | -19, -19 |
Flurbiprofen (FPN) | 8.10 | 243.1 | 198.9*, 178.7 | -30, -30 | -12, -12 |
Diclofenacacid (DCF) | 8.42 | 294.3 | 249.8*, 213.7 | -48, -48 | -15, -15 |
Ibuprofen (IBF) | 8.71 | 205.0 | 161.0*, 159.2 | -40, -40 | -12, -9 |
Table 1 MS parameters of the five nonsteroidal anti-inflammatory drugs (NSAIDS)
Analyte | tR/min | Precursor ion (m/z) | Product ions (m/z) | Declustering potentials/V | Collision energies/eV |
---|---|---|---|---|---|
Ketoprofen (KPF) | 6.44 | 253.0 | 209.0*, 197.0 | -36, -36 | -8, -19 |
Naproxen (NPX) | 6.73 | 229.3 | 169.8*, 184.8 | -38, -38 | -19, -19 |
Flurbiprofen (FPN) | 8.10 | 243.1 | 198.9*, 178.7 | -30, -30 | -12, -12 |
Diclofenacacid (DCF) | 8.42 | 294.3 | 249.8*, 213.7 | -48, -48 | -15, -15 |
Ibuprofen (IBF) | 8.71 | 205.0 | 161.0*, 159.2 | -40, -40 | -12, -9 |
Fig. 2 SEM images of Co-UiO-67(bpy) and Co-UiO-67(bpy)/CS a. Co-UiO-67(bpy) (magnification of 100000); b, c, d. Co-UiO-67(bpy)/CS (magnifications of 1000, 5000, 50000).
Fig. 6 Effects of (a) types of extraction material, (b) amounts of MOFs, (c) extraction time, (d) values of sample pH, (e) ionic strength, (f) volume fractions of formic acid, (g) volumes of eluent, and (h) elution time on the extraction effects of the five NSAIDs (n=3) MOFs: metal-organic frameworks.
Analyte | Linear equation | r2 | Linear range/(ng/L) | LOD/(ng/L) | LOQ/(ng/L) |
---|---|---|---|---|---|
KPF | y=3.89×102x+1.68×103 | 0.9986 | 10-2000 | 0.32 | 1.05 |
NPX | y=7.07×102x+3.52×102 | 0.9982 | 5-2000 | 2.06 | 6.78 |
FPN | y=9.34×101x+6.17×102 | 0.9964 | 10-2000 | 1.21 | 3.97 |
DCF | y=1.27×102x+2.01×103 | 0.9937 | 5-2000 | 0.70 | 2.32 |
IBF | y=4.71×101x+7.74×102 | 0.9993 | 10-2000 | 1.51 | 4.97 |
Table 2 Linear equations, correlation coefficients (r2), linear ranges, LODs and LOQs of the five NSAIDs
Analyte | Linear equation | r2 | Linear range/(ng/L) | LOD/(ng/L) | LOQ/(ng/L) |
---|---|---|---|---|---|
KPF | y=3.89×102x+1.68×103 | 0.9986 | 10-2000 | 0.32 | 1.05 |
NPX | y=7.07×102x+3.52×102 | 0.9982 | 5-2000 | 2.06 | 6.78 |
FPN | y=9.34×101x+6.17×102 | 0.9964 | 10-2000 | 1.21 | 3.97 |
DCF | y=1.27×102x+2.01×103 | 0.9937 | 5-2000 | 0.70 | 2.32 |
IBF | y=4.71×101x+7.74×102 | 0.9993 | 10-2000 | 1.51 | 4.97 |
Analyte | Spiked/ (ng/L) | Recovery/ % | RSDs/% | |
---|---|---|---|---|
Intra-day | Inter-day | |||
KPF | 40 | 78.9 | 8.8 | 11.0 |
250 | 107.9 | 9.4 | 8.6 | |
1500 | 89.1 | 6.6 | 11.2 | |
NPX | 40 | 82.9 | 7.1 | 1.3 |
250 | 87.0 | 3.8 | 10.6 | |
1500 | 92.6 | 3.3 | 9.8 | |
FPN | 40 | 114.1 | 5.1 | 6.1 |
250 | 100.4 | 10.7 | 9.2 | |
1500 | 101.0 | 5.3 | 6.6 | |
DCF | 40 | 74.5 | 2.5 | 11.5 |
250 | 97.8 | 11.7 | 8.3 | |
1500 | 104.7 | 12.3 | 10.3 | |
IBF | 40 | 79.7 | 1.3 | 4.5 |
250 | 83.7 | 5.0 | 8.7 | |
1500 | 89.6 | 6.1 | 8.8 |
Table 3 Spiked recoveries and precisions of the five NSAIDs (n=6)
Analyte | Spiked/ (ng/L) | Recovery/ % | RSDs/% | |
---|---|---|---|---|
Intra-day | Inter-day | |||
KPF | 40 | 78.9 | 8.8 | 11.0 |
250 | 107.9 | 9.4 | 8.6 | |
1500 | 89.1 | 6.6 | 11.2 | |
NPX | 40 | 82.9 | 7.1 | 1.3 |
250 | 87.0 | 3.8 | 10.6 | |
1500 | 92.6 | 3.3 | 9.8 | |
FPN | 40 | 114.1 | 5.1 | 6.1 |
250 | 100.4 | 10.7 | 9.2 | |
1500 | 101.0 | 5.3 | 6.6 | |
DCF | 40 | 74.5 | 2.5 | 11.5 |
250 | 97.8 | 11.7 | 8.3 | |
1500 | 104.7 | 12.3 | 10.3 | |
IBF | 40 | 79.7 | 1.3 | 4.5 |
250 | 83.7 | 5.0 | 8.7 | |
1500 | 89.6 | 6.1 | 8.8 |
Material | Method | Matrices | Extraction time/min | Practicable pH | LOD/ (ng/L) | Ref. |
---|---|---|---|---|---|---|
Fe3O4@/MIL-101(Cr) | MSPE-UPLC-MS/MS | waste water | 18 | 5 | 3.00-60.00 | [1] |
MIL-101(Cr)/PVA | VA-SPE-HPLC-MS/MS | river, pharmaceutical, | 60 | 4 | 7.00-37.00 | [33] |
waste and feed water | ||||||
Fe3O4@MIL-100(Fe) | MSPE-UPLC-MS/MS | feed, waste, lake and | 60 | 5 | 20.00-90.00 | [34] |
pharmaceutical water | ||||||
C18 | SPE-HPLC-MS/MS | surface water | >80 | 3 | 0.01-0.07 | [35] |
MIL-101(Cr)@GA | SPE-UPLC-MS/MS | river, lake and waste water | 30 | 4 | 6.00-12.00 | [36] |
PANI/Pan NFsM | SPE-UPLC-MS/MS | drinking water | >20 | 7 | 0.40-5.00 | [37] |
Co-UiO-67(bpy)/CS | DSPE-UPLC-MS/MS | reservoir and waste water | 11 | 6 | 0.32-2.06 | this work |
Table 4 Comparison of the present method with the reported methods for the determination of NSAIDs
Material | Method | Matrices | Extraction time/min | Practicable pH | LOD/ (ng/L) | Ref. |
---|---|---|---|---|---|---|
Fe3O4@/MIL-101(Cr) | MSPE-UPLC-MS/MS | waste water | 18 | 5 | 3.00-60.00 | [1] |
MIL-101(Cr)/PVA | VA-SPE-HPLC-MS/MS | river, pharmaceutical, | 60 | 4 | 7.00-37.00 | [33] |
waste and feed water | ||||||
Fe3O4@MIL-100(Fe) | MSPE-UPLC-MS/MS | feed, waste, lake and | 60 | 5 | 20.00-90.00 | [34] |
pharmaceutical water | ||||||
C18 | SPE-HPLC-MS/MS | surface water | >80 | 3 | 0.01-0.07 | [35] |
MIL-101(Cr)@GA | SPE-UPLC-MS/MS | river, lake and waste water | 30 | 4 | 6.00-12.00 | [36] |
PANI/Pan NFsM | SPE-UPLC-MS/MS | drinking water | >20 | 7 | 0.40-5.00 | [37] |
Co-UiO-67(bpy)/CS | DSPE-UPLC-MS/MS | reservoir and waste water | 11 | 6 | 0.32-2.06 | this work |
Analyte | Spiked/ (ng/L) | Reservoir water | Waste water | |||||
---|---|---|---|---|---|---|---|---|
Found/(ng/L) | Recovery/% | RSD/% | Found/(ng/L) | Recovery/% | RSD/% | |||
KPF | 0 | ND | 14.52 | |||||
40 | 44.25 | 110.6 | 11.9 | 55.85 | 103.3 | 12.6 | ||
250 | 243.70 | 93.9 | 10.2 | 259.51 | 98.0 | 7.9 | ||
1500 | 1103.83 | 73.6 | 6.9 | 1060.06 | 69.7 | 0.1 | ||
NPX | 0 | ND | ND | |||||
40 | 42.47 | 106.2 | 6.8 | 37.23 | 93.1 | 2.1 | ||
250 | 203.12 | 81.3 | 5.9 | 201.08 | 80.4 | 7.3 | ||
1500 | 1524.74 | 101.7 | 7.7 | 1253.34 | 83.6 | 4.8 | ||
FPN | 0 | ND | 10.05 | |||||
40 | 45.24 | 113.1 | 6.0 | 42.47 | 81.0 | 3.1 | ||
250 | 239.73 | 95.9 | 2.5 | 250.77 | 96.3 | 3.9 | ||
1500 | 1525.16 | 101.7 | 5.9 | 1403.86 | 92.9 | 12.0 | ||
DCF | 0 | ND | ND | |||||
40 | 33.60 | 84.0 | 2.8 | 33.97 | 84.9 | 5.6 | ||
250 | 190.50 | 76.2 | 5.4 | 219.08 | 87.6 | 5.4 | ||
1500 | 1488.03 | 99.2 | 10.9 | 1291.94 | 86.1 | 1.3 | ||
IBF | 0 | ND | ND | |||||
40 | 37.32 | 93.3 | 1.3 | 41.89 | 104.7 | 5.3 | ||
250 | 186.57 | 74.6 | 1.4 | 193.62 | 77.4 | 9.3 | ||
1500 | 1341.46 | 89.4 | 0.6 | 1108.73 | 73.9 | 2.4 |
Table 5 Analytical results of the five NSAIDs in real water samples (n=3)
Analyte | Spiked/ (ng/L) | Reservoir water | Waste water | |||||
---|---|---|---|---|---|---|---|---|
Found/(ng/L) | Recovery/% | RSD/% | Found/(ng/L) | Recovery/% | RSD/% | |||
KPF | 0 | ND | 14.52 | |||||
40 | 44.25 | 110.6 | 11.9 | 55.85 | 103.3 | 12.6 | ||
250 | 243.70 | 93.9 | 10.2 | 259.51 | 98.0 | 7.9 | ||
1500 | 1103.83 | 73.6 | 6.9 | 1060.06 | 69.7 | 0.1 | ||
NPX | 0 | ND | ND | |||||
40 | 42.47 | 106.2 | 6.8 | 37.23 | 93.1 | 2.1 | ||
250 | 203.12 | 81.3 | 5.9 | 201.08 | 80.4 | 7.3 | ||
1500 | 1524.74 | 101.7 | 7.7 | 1253.34 | 83.6 | 4.8 | ||
FPN | 0 | ND | 10.05 | |||||
40 | 45.24 | 113.1 | 6.0 | 42.47 | 81.0 | 3.1 | ||
250 | 239.73 | 95.9 | 2.5 | 250.77 | 96.3 | 3.9 | ||
1500 | 1525.16 | 101.7 | 5.9 | 1403.86 | 92.9 | 12.0 | ||
DCF | 0 | ND | ND | |||||
40 | 33.60 | 84.0 | 2.8 | 33.97 | 84.9 | 5.6 | ||
250 | 190.50 | 76.2 | 5.4 | 219.08 | 87.6 | 5.4 | ||
1500 | 1488.03 | 99.2 | 10.9 | 1291.94 | 86.1 | 1.3 | ||
IBF | 0 | ND | ND | |||||
40 | 37.32 | 93.3 | 1.3 | 41.89 | 104.7 | 5.3 | ||
250 | 186.57 | 74.6 | 1.4 | 193.62 | 77.4 | 9.3 | ||
1500 | 1341.46 | 89.4 | 0.6 | 1108.73 | 73.9 | 2.4 |
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