Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (8): 704-711.DOI: 10.3724/SP.J.1123.2022.03017
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LI Hui1, REN Gengbiao2, LI Huijuan2, CHEN Xiangfeng2, ZHANG Zhiguo1, ZHAO Yanfang2,*()
Received:
2022-03-11
Online:
2022-08-08
Published:
2022-07-29
Contact:
ZHAO Yanfang
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CLC Number:
LI Hui, REN Gengbiao, LI Huijuan, CHEN Xiangfeng, ZHANG Zhiguo, ZHAO Yanfang. Imine-linked porous covalent organic framework used for the solid-phase extraction of estrogens from honey prior to liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(8): 704-711.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.03017
Compound | Formula | tR/min | Precursor ion (m/z) | Fragment ion (m/z) | Clustering voltage/V | Collision energy/V |
---|---|---|---|---|---|---|
E3 | C18H24O3 | 0.90 | 286.9 | 144.8 | -110 | -47 |
170.9 | -110 | -45 | ||||
E2 | C18H24O2 | 1.68 | 270.9 | 145.0 | -100 | -57 |
182.8 | -100 | -45 | ||||
EE2 | C20H24O2 | 2.02 | 295.0 | 144.8 | -110 | -50 |
269.0 | -110 | -50 | ||||
E1 | C18H24O2 | 2.25 | 266.8 | 250.9 | -100 | -40 |
236.8 | -100 | -40 | ||||
DES | C18H20O2 | 2.60 | 272.8 | 185.0 | -100 | -57 |
147.0 | -100 | -50 |
Table 1 Multiple reaction-monitoring (MRM) mode parameters of estrogens
Compound | Formula | tR/min | Precursor ion (m/z) | Fragment ion (m/z) | Clustering voltage/V | Collision energy/V |
---|---|---|---|---|---|---|
E3 | C18H24O3 | 0.90 | 286.9 | 144.8 | -110 | -47 |
170.9 | -110 | -45 | ||||
E2 | C18H24O2 | 1.68 | 270.9 | 145.0 | -100 | -57 |
182.8 | -100 | -45 | ||||
EE2 | C20H24O2 | 2.02 | 295.0 | 144.8 | -110 | -50 |
269.0 | -110 | -50 | ||||
E1 | C18H24O2 | 2.25 | 266.8 | 250.9 | -100 | -40 |
236.8 | -100 | -40 | ||||
DES | C18H20O2 | 2.60 | 272.8 | 185.0 | -100 | -57 |
147.0 | -100 | -50 |
Fig. 1 Characterization of imine-linked porous covalent organic framework material (IL-COF-1) a. SEM image; b. TEM image; c. X-ray diffraction (XRD) patterns; d. nitrogen adsorption/desorption isotherms; e. pore size distribution curves; f. FT-IR spectrum.
Fig. 2 Effects of (a) IL-COF-1 amount, (b) sample pH, (c) sample flow rate, (d) eluent volume, (e) flow rate of eluent, and (f) NaCl concentration on estrogen extraction efficiency (n=6)
Fig. 3 Effect of eluent type on estrogen extraction efficiency (n=6) 1. methanol; 2. acetonitrile; 3. ethyl acetate; 4. 1% (v/v) NH3·H2O-methanol; 5. 1% (v/v) NH3·H2O-acetonitrile; 6. 1% (v/v) NH3·H2O-ethyl acetate.
Compound | Linear range/(ng/g) | Correlation coefficient (r) | LOD/(ng/g) | LOQ/(ng/g) | RSDs/% (n=5) | |
---|---|---|---|---|---|---|
Intra-day | Inter-day | |||||
E3 | 1-500 | 0.9934 | 0.25 | 0.80 | 4.4 | 6.7 |
E2 | 1-500 | 0.9955 | 0.25 | 0.80 | 6.6 | 7.9 |
EE2 | 1-500 | 0.9967 | 0.30 | 0.95 | 5.2 | 5.7 |
E1 | 0.1-100 | 0.9972 | 0.02 | 0.07 | 3.2 | 4.6 |
DES | 0.1-100 | 0.9966 | 0.01 | 0.05 | 5.4 | 4.2 |
Table 2 Analytical parameters of SPE-HPLC-MS/MS method
Compound | Linear range/(ng/g) | Correlation coefficient (r) | LOD/(ng/g) | LOQ/(ng/g) | RSDs/% (n=5) | |
---|---|---|---|---|---|---|
Intra-day | Inter-day | |||||
E3 | 1-500 | 0.9934 | 0.25 | 0.80 | 4.4 | 6.7 |
E2 | 1-500 | 0.9955 | 0.25 | 0.80 | 6.6 | 7.9 |
EE2 | 1-500 | 0.9967 | 0.30 | 0.95 | 5.2 | 5.7 |
E1 | 0.1-100 | 0.9972 | 0.02 | 0.07 | 3.2 | 4.6 |
DES | 0.1-100 | 0.9966 | 0.01 | 0.05 | 5.4 | 4.2 |
Estrogen | Added level/(ng/g) | Recoveries/% | |||
---|---|---|---|---|---|
Linden honey 1 | Linden honey 2 | Acacia honey 1 | Acacia honey 2 | ||
E3 | 5 | 85.22±2.56 | 83.16±3.36 | 95.22±2.56 | 88.56±2.25 |
25 | 88.96±4.25 | 86.97±4.14 | 88.52±3.65 | 89.67±4.21 | |
50 | 93.26±2.14 | 91.24±5.14 | 85.25±2.24 | 95.62±5.32 | |
E2 | 5 | 102.52±4.57 | 85.66±4.21 | 99.58±3.33 | 89.64±2.28 |
25 | 95.62±3.22 | 94.25±3.55 | 92.25±4.24 | 99.63±1.65 | |
50 | 107.32±3.54 | 97.45±4.14 | 87.42±1.15 | 87.58±4.15 | |
EE2 | 5 | 86.45±4.78 | 97.36±5.21 | 87.66±4.41 | 92.35±2.27 |
25 | 96.33±3.68 | 87.55±4.78 | 80.14±2.22 | 96.35±3.45 | |
50 | 85.67±4.58 | 99.25±4.57 | 86.35±4.25 | 90.24±2.27 | |
E1 | 5 | 101.51±4.77 | 85.24±2.41 | 86.66±3.32 | 115.24±4.24 |
25 | 83.24±3.98 | 88.44±2.57 | 88.57±2.26 | 87.36±3.56 | |
50 | 103.64±4.44 | 99.64±1.11 | 97.25±1.18 | 95.31±4.21 | |
DES | 5 | 86.53±3.89 | 87.21±2.25 | 97.58±2.26 | 88.65±4.21 |
25 | 85.32±4.57 | 88.57±3.58 | 102.33±5.22 | 86.31±4.15 | |
50 | 95.51±4.67 | 96.80±4.22 | 103.52±3.31 | 99.65±3.67 |
Table 3 Spiked recoveries of the five estrogens in honey samples (n=5)
Estrogen | Added level/(ng/g) | Recoveries/% | |||
---|---|---|---|---|---|
Linden honey 1 | Linden honey 2 | Acacia honey 1 | Acacia honey 2 | ||
E3 | 5 | 85.22±2.56 | 83.16±3.36 | 95.22±2.56 | 88.56±2.25 |
25 | 88.96±4.25 | 86.97±4.14 | 88.52±3.65 | 89.67±4.21 | |
50 | 93.26±2.14 | 91.24±5.14 | 85.25±2.24 | 95.62±5.32 | |
E2 | 5 | 102.52±4.57 | 85.66±4.21 | 99.58±3.33 | 89.64±2.28 |
25 | 95.62±3.22 | 94.25±3.55 | 92.25±4.24 | 99.63±1.65 | |
50 | 107.32±3.54 | 97.45±4.14 | 87.42±1.15 | 87.58±4.15 | |
EE2 | 5 | 86.45±4.78 | 97.36±5.21 | 87.66±4.41 | 92.35±2.27 |
25 | 96.33±3.68 | 87.55±4.78 | 80.14±2.22 | 96.35±3.45 | |
50 | 85.67±4.58 | 99.25±4.57 | 86.35±4.25 | 90.24±2.27 | |
E1 | 5 | 101.51±4.77 | 85.24±2.41 | 86.66±3.32 | 115.24±4.24 |
25 | 83.24±3.98 | 88.44±2.57 | 88.57±2.26 | 87.36±3.56 | |
50 | 103.64±4.44 | 99.64±1.11 | 97.25±1.18 | 95.31±4.21 | |
DES | 5 | 86.53±3.89 | 87.21±2.25 | 97.58±2.26 | 88.65±4.21 |
25 | 85.32±4.57 | 88.57±3.58 | 102.33±5.22 | 86.31±4.15 | |
50 | 95.51±4.67 | 96.80±4.22 | 103.52±3.31 | 99.65±3.67 |
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