Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (2): 198-205.DOI: 10.3724/SP.J.1123.2021.05009
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WANG Xueting1,*(), LI Jingjing1, JIANG Shan1, SHEN Weijian1, WANG Yiqian1, GU Qiang2
Received:
2021-05-14
Online:
2022-02-08
Published:
2022-01-26
Contact:
WANG Xueting
Supported by:
CLC Number:
WANG Xueting, LI Jingjing, JIANG Shan, SHEN Weijian, WANG Yiqian, GU Qiang. Simultaneous determination of monochloropropanediol esters and glycidyl esters in vegetable oils by acidic transesterification-gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40(2): 198-205.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.05009
Target compound | Retention time/min | Quantitative ion (m/z) | Qualitative ions (m/z) |
---|---|---|---|
3-MCPD-PBA | 10.960 | 147 | 91, 196 |
D5-3-MCPD-PBA | 10.898 | 203 | 93, 150 |
2-MCPD-PBA | 11.561 | 198 | 104, 196 |
D5-2-MCPD-PBA | 11.488 | 201 | 93, 104 |
3-MBPD-PBA | 12.885 | 240 | 91, 146 |
D5-3-MBPD-PBA | 12.795 | 245 | 149, 150 |
Table 1 Retention times, quantitative and qualitative ions of the three target compounds and their internal standards (IS)
Target compound | Retention time/min | Quantitative ion (m/z) | Qualitative ions (m/z) |
---|---|---|---|
3-MCPD-PBA | 10.960 | 147 | 91, 196 |
D5-3-MCPD-PBA | 10.898 | 203 | 93, 150 |
2-MCPD-PBA | 11.561 | 198 | 104, 196 |
D5-2-MCPD-PBA | 11.488 | 201 | 93, 104 |
3-MBPD-PBA | 12.885 | 240 | 91, 146 |
D5-3-MBPD-PBA | 12.795 | 245 | 149, 150 |
Fig. 1 Total ion current chromatograms and mass spectra of the three target compounds and their IS The concentrations of the three target substances were 10 mg/L, and the concentrations of their IS were 5 mg/L.
Fig. 2 Effect of (a) bromination reaction temperature and bromination reaction time (b) on the conversion efficiency of IS D5-glycidyl palmitate in vegetable oil samples
Fig. 3 Effect of (a) volume of derivatization reagent and (b) derivatization reaction time on the determination results of three IS in vegetable oil samples
Compound | Linear equation | r2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|
3-MCPD-PBA | y=17.770068x-0.196156 | 0.9998 | 25 | 75 |
2-MCPD-PBA | y=0.391145x+0.001431 | 0.9998 | 25 | 75 |
3-MBPD-PBA | y=0.722427x-0.007760 | 0.9999 | 20 | 60 |
Table 2 Linear equations, correlation coefficients (r2), limits of detection (LODs) and limits of quantification (LOQs) of target compounds
Compound | Linear equation | r2 | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|
3-MCPD-PBA | y=17.770068x-0.196156 | 0.9998 | 25 | 75 |
2-MCPD-PBA | y=0.391145x+0.001431 | 0.9998 | 25 | 75 |
3-MBPD-PBA | y=0.722427x-0.007760 | 0.9999 | 20 | 60 |
Oil type | Spiked/ (μg/kg) | 3-MCPDEs | 2-MCPDEs | GEs | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Measured/ (mg/kg) | Recovery/ % | RSD/% | Measured/ (mg/kg) | Recovery/ % | RSD/ % | Measured/ (mg/kg) | Recovery/ % | RSD/ % | ||||
Soybean oil | 0 | ND | - | - | ND | - | - | ND | - | - | ||
250 | 0.244±0.015 | 89.3 | 5.98 | 0.258±0.012 | 89.0 | 4.60 | 0.274±0.014 | 90.3 | 4.94 | |||
500 | 0.478±0.019 | 91.8 | 3.98 | 0.505±0.017 | 94.3 | 3.33 | 0.523±0.019 | 95.2 | 3.72 | |||
750 | 0.736±0.018 | 95.9 | 2.44 | 0.740±0.018 | 94.5 | 2.37 | 0.758±0.017 | 95.2 | 2.26 | |||
Rapeseed oil | 0 | 0.216±0.014 | - | 6.37 | 0.117±0.009 | - | 7.81 | 0.409±0.017 | - | 4.21 | ||
250 | 0.439±0.018 | 90.0 | 4.02 | 0.351±0.015 | 94.4 | 4.16 | 0.644±0.020 | 94.6 | 3.15 | |||
500 | 0.677±0.025 | 92.8 | 3.71 | 0.578±0.019 | 92.9 | 3.31 | 0.869±0.025 | 92.6 | 2.92 | |||
750 | 0.931±0.027 | 96.1 | 2.91 | 0.840±0.020 | 97.2 | 2.39 | 1.144±0.028 | 98.7 | 2.43 | |||
Sunflower oil | 0 | ND | - | - | ND | - | - | 0.107±0.003 | - | 2.93 | ||
250 | 0.240±0.010 | 91.7 | 4.21 | 0.258±0.010 | 90.9 | 3.91 | 0.335±0.013 | 91.9 | 3.79 | |||
500 | 0.476±0.019 | 93.5 | 4.08 | 0.487±0.019 | 91.5 | 3.86 | 0.573±0.019 | 93.9 | 3.23 | |||
750 | 0.725±0.016 | 96.1 | 2.26 | 0.764±0.017 | 98.7 | 2.17 | 0.809±0.025 | 94.8 | 3.15 | |||
Linseed oil | 0 | ND | - | - | ND | - | - | ND | - | - | ||
250 | 0.243±0.013 | 91.3 | 5.49 | 0.247±0.010 | 91.0 | 4.22 | 0.256±0.013 | 91.3 | 5.22 | |||
500 | 0.483±0.021 | 94.0 | 4.27 | 0.488±0.018 | 94.0 | 3.76 | 0.493±0.019 | 93.5 | 3.93 | |||
750 | 0.744±0.019 | 97.6 | 2.53 | 0.736±0.015 | 95.9 | 2.05 | 0.740±0.017 | 95.4 | 2.35 |
Table 3 Spiked recoveries and RSDs of 3-MCPDEs, 2-MCPDEs and GEs in vegetable oils (n=6)
Oil type | Spiked/ (μg/kg) | 3-MCPDEs | 2-MCPDEs | GEs | ||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|
Measured/ (mg/kg) | Recovery/ % | RSD/% | Measured/ (mg/kg) | Recovery/ % | RSD/ % | Measured/ (mg/kg) | Recovery/ % | RSD/ % | ||||
Soybean oil | 0 | ND | - | - | ND | - | - | ND | - | - | ||
250 | 0.244±0.015 | 89.3 | 5.98 | 0.258±0.012 | 89.0 | 4.60 | 0.274±0.014 | 90.3 | 4.94 | |||
500 | 0.478±0.019 | 91.8 | 3.98 | 0.505±0.017 | 94.3 | 3.33 | 0.523±0.019 | 95.2 | 3.72 | |||
750 | 0.736±0.018 | 95.9 | 2.44 | 0.740±0.018 | 94.5 | 2.37 | 0.758±0.017 | 95.2 | 2.26 | |||
Rapeseed oil | 0 | 0.216±0.014 | - | 6.37 | 0.117±0.009 | - | 7.81 | 0.409±0.017 | - | 4.21 | ||
250 | 0.439±0.018 | 90.0 | 4.02 | 0.351±0.015 | 94.4 | 4.16 | 0.644±0.020 | 94.6 | 3.15 | |||
500 | 0.677±0.025 | 92.8 | 3.71 | 0.578±0.019 | 92.9 | 3.31 | 0.869±0.025 | 92.6 | 2.92 | |||
750 | 0.931±0.027 | 96.1 | 2.91 | 0.840±0.020 | 97.2 | 2.39 | 1.144±0.028 | 98.7 | 2.43 | |||
Sunflower oil | 0 | ND | - | - | ND | - | - | 0.107±0.003 | - | 2.93 | ||
250 | 0.240±0.010 | 91.7 | 4.21 | 0.258±0.010 | 90.9 | 3.91 | 0.335±0.013 | 91.9 | 3.79 | |||
500 | 0.476±0.019 | 93.5 | 4.08 | 0.487±0.019 | 91.5 | 3.86 | 0.573±0.019 | 93.9 | 3.23 | |||
750 | 0.725±0.016 | 96.1 | 2.26 | 0.764±0.017 | 98.7 | 2.17 | 0.809±0.025 | 94.8 | 3.15 | |||
Linseed oil | 0 | ND | - | - | ND | - | - | ND | - | - | ||
250 | 0.243±0.013 | 91.3 | 5.49 | 0.247±0.010 | 91.0 | 4.22 | 0.256±0.013 | 91.3 | 5.22 | |||
500 | 0.483±0.021 | 94.0 | 4.27 | 0.488±0.018 | 94.0 | 3.76 | 0.493±0.019 | 93.5 | 3.93 | |||
750 | 0.744±0.019 | 97.6 | 2.53 | 0.736±0.015 | 95.9 | 2.05 | 0.740±0.017 | 95.4 | 2.35 |
Analyte | Assigned value/ (mg/kg) | Contents/(mg/kg) | ||
---|---|---|---|---|
This method | GB 5009.191-2016 | SN/T 5220-2019 | ||
3-MCPDEs | 0.569 | 0.558±0.016 | 0.498±0.033 | 0.516±0.031 |
2-MCPDEs | 0.275 | 0.265±0.012 | 0.211±0.024 | - |
GEs | 0.459 | 0.456±0.015 | - | - |
Table 4 Contents of three target substances in vegetable oil by different methods (n=6)
Analyte | Assigned value/ (mg/kg) | Contents/(mg/kg) | ||
---|---|---|---|---|
This method | GB 5009.191-2016 | SN/T 5220-2019 | ||
3-MCPDEs | 0.569 | 0.558±0.016 | 0.498±0.033 | 0.516±0.031 |
2-MCPDEs | 0.275 | 0.265±0.012 | 0.211±0.024 | - |
GEs | 0.459 | 0.456±0.015 | - | - |
Oil type | Sample number | Contents/(mg/kg) | ||
---|---|---|---|---|
3-MCPDEs | 2-MCPDEs | GEs | ||
Soybean oil | 22 | ND-0.970 | ND-0.456 | ND-1.600 |
Rapeseed oil | 40 | ND-1.292 | ND-0.549 | ND-2.177 |
Sunflower oil | 16 | ND-0.398 | ND-0.219 | ND-0.505 |
Corn oil | 12 | 0.068-0.509 | 0.089-0.498 | 0.108-0.639 |
Sesame oil | 22 | 0.223-3.670 | 0.109-1.550 | 0.059-1.720 |
Table 5 Detected results of 3-MCPDEs, 2-MCPDEs and GEs in real samples
Oil type | Sample number | Contents/(mg/kg) | ||
---|---|---|---|---|
3-MCPDEs | 2-MCPDEs | GEs | ||
Soybean oil | 22 | ND-0.970 | ND-0.456 | ND-1.600 |
Rapeseed oil | 40 | ND-1.292 | ND-0.549 | ND-2.177 |
Sunflower oil | 16 | ND-0.398 | ND-0.219 | ND-0.505 |
Corn oil | 12 | 0.068-0.509 | 0.089-0.498 | 0.108-0.639 |
Sesame oil | 22 | 0.223-3.670 | 0.109-1.550 | 0.059-1.720 |
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