Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (12): 1095-1101.DOI: 10.3724/SP.J.1123.2022.03006
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ZOU You, SHAO Linzhi(), LAN Cao, CHEN Simin
Received:
2022-03-10
Online:
2022-12-08
Published:
2022-11-29
Contact:
SHAO Linzhi
CLC Number:
ZOU You, SHAO Linzhi, LAN Cao, CHEN Simin. Simultaneous determination of three components of sodium nitrophenolate in foodstuffs of animal origin by high performance liquid chromatography-tandem mass spectrometry using atmospheric pressure chemical ionization[J]. Chinese Journal of Chromatography, 2022, 40(12): 1095-1101.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.03006
Compound | tR/min | Parent ion (m/z) | Product ions (m/z) | DP/V | CEs/eV |
---|---|---|---|---|---|
5-Nitroguaiacol sodium (5NG) | 4.89 | 168.0 | 153.0*, 123.0 | -55 | -18, -27 |
4-Nitrophenol sodium (PNP) | 4.96 | 138.0 | 108.0*, 92.0 | -90 | -20, -23 |
2-Nitrophenol sodium (ONP) | 5.82 | 138.0 | 108.0*, 92.0 | -90 | -22, -30 |
Table 1 Retention times and MS/MS parameters for 5NG, PNP and ONP in MRM mode
Compound | tR/min | Parent ion (m/z) | Product ions (m/z) | DP/V | CEs/eV |
---|---|---|---|---|---|
5-Nitroguaiacol sodium (5NG) | 4.89 | 168.0 | 153.0*, 123.0 | -55 | -18, -27 |
4-Nitrophenol sodium (PNP) | 4.96 | 138.0 | 108.0*, 92.0 | -90 | -20, -23 |
2-Nitrophenol sodium (ONP) | 5.82 | 138.0 | 108.0*, 92.0 | -90 | -22, -30 |
Fig. 2 Total ion chromatograms of 5NG, PNP and ONP in mixed standard solutions at atmospheric pressure chemical ionization mode 5NG: 10 μg/L; PNP: 20 μg/L; ONP: 50 μg/L.
Compound | Regression equation | Linear range/(μg/L) | r2 | LOQ/(μg/kg) |
---|---|---|---|---|
5NG | Y=1.90×105X-6.27×103 | 0.5-10 | 0.99999 | 1.0 |
PNP | Y=2.32×105X+1.30×105 | 1.0-20 | 0.99998 | 2.0 |
ONP | Y=4.54×104X+3.77×103 | 2.5-50 | 0.99991 | 5.0 |
Table 2 Regression equations, linear ranges, correlation coefficients (r2), and limits of quantification (LOQs) of 5NG, PNP and ONP
Compound | Regression equation | Linear range/(μg/L) | r2 | LOQ/(μg/kg) |
---|---|---|---|---|
5NG | Y=1.90×105X-6.27×103 | 0.5-10 | 0.99999 | 1.0 |
PNP | Y=2.32×105X+1.30×105 | 1.0-20 | 0.99998 | 2.0 |
ONP | Y=4.54×104X+3.77×103 | 2.5-50 | 0.99991 | 5.0 |
Compound | Added/ (μg/kg) | Pork | Fish | Chicken | Liver | ||||
---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||
5NG | 1.0 | 95.0 | 5.98 | 88.6 | 3.20 | 85.4 | 2.74 | 84.6 | 2.70 |
2.0 | 92.0 | 5.30 | 82.8 | 1.51 | 81.6 | 1.75 | 83.0 | 2.10 | |
10.0 | 98.4 | 3.79 | 82.8 | 1.87 | 81.5 | 1.87 | 84.1 | 4.06 | |
PNP | 2.0 | 100 | 5.17 | 88.0 | 8.85 | 83.3 | 1.11 | 92.3 | 1.82 |
4.0 | 101 | 2.77 | 84.3 | 2.34 | 87.1 | 3.81 | 84.5 | 2.65 | |
20.0 | 102 | 1.70 | 81.5 | 1.86 | 86.9 | 2.62 | 85.6 | 2.83 | |
ONP | 5.0 | 95.1 | 8.61 | 90.6 | 1.95 | 82.8 | 0.91 | 87.3 | 5.90 |
10.0 | 84.8 | 5.88 | 83.3 | 2.77 | 84.9 | 1.78 | 83.7 | 2.93 | |
50.0 | 85.5 | 4.85 | 82.1 | 1.82 | 83.6 | 2.63 | 81.4 | 1.39 |
Table 3 Spiked recoveries and RSDs of 5NG, PNP and ONP in pork, chicken, fish and liver samples (n=6)
Compound | Added/ (μg/kg) | Pork | Fish | Chicken | Liver | ||||
---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||
5NG | 1.0 | 95.0 | 5.98 | 88.6 | 3.20 | 85.4 | 2.74 | 84.6 | 2.70 |
2.0 | 92.0 | 5.30 | 82.8 | 1.51 | 81.6 | 1.75 | 83.0 | 2.10 | |
10.0 | 98.4 | 3.79 | 82.8 | 1.87 | 81.5 | 1.87 | 84.1 | 4.06 | |
PNP | 2.0 | 100 | 5.17 | 88.0 | 8.85 | 83.3 | 1.11 | 92.3 | 1.82 |
4.0 | 101 | 2.77 | 84.3 | 2.34 | 87.1 | 3.81 | 84.5 | 2.65 | |
20.0 | 102 | 1.70 | 81.5 | 1.86 | 86.9 | 2.62 | 85.6 | 2.83 | |
ONP | 5.0 | 95.1 | 8.61 | 90.6 | 1.95 | 82.8 | 0.91 | 87.3 | 5.90 |
10.0 | 84.8 | 5.88 | 83.3 | 2.77 | 84.9 | 1.78 | 83.7 | 2.93 | |
50.0 | 85.5 | 4.85 | 82.1 | 1.82 | 83.6 | 2.63 | 81.4 | 1.39 |
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