Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (3): 316-323.DOI: 10.3724/SP.J.1123.2020.06007
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YAN Meng, JIA Yeqing, QI Peiru, WANG Yahui, JI Qianqian, WANG Manman, WANG Qian, HAO Yulan*()
Received:
2020-06-03
Online:
2021-03-08
Published:
2021-02-03
Contact:
HAO Yulan
Supported by:
CLC Number:
YAN Meng, JIA Yeqing, QI Peiru, WANG Yahui, JI Qianqian, WANG Manman, WANG Qian, HAO Yulan. Determination of three diphenyl ether herbicides in rice by magnetic solid phase extraction using Fe3O4@MOF-808 coupled with high performance liquid chromatography[J]. Chinese Journal of Chromatography, 2021, 39(3): 316-323.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.06007
Analyte | Linear range/ (μg/L) | Regression equation | r | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|
BIF | 2-300 | y=56.804x-1.0564 | 0.9992 | 0.4 | 1.5 |
OXY | 2-300 | y=52.783x-0.3415 | 0.9991 | 0.6 | 2.0 |
NIT | 2-300 | y=55.413x+0.0566 | 0.9984 | 0.6 | 2.0 |
Table 1 Linear ranges, LODs and LOQs of the three Des
Analyte | Linear range/ (μg/L) | Regression equation | r | LOD/ (μg/kg) | LOQ/ (μg/kg) |
---|---|---|---|---|---|
BIF | 2-300 | y=56.804x-1.0564 | 0.9992 | 0.4 | 1.5 |
OXY | 2-300 | y=52.783x-0.3415 | 0.9991 | 0.6 | 2.0 |
NIT | 2-300 | y=55.413x+0.0566 | 0.9984 | 0.6 | 2.0 |
Analyte | Spiked/ (μg/kg) | Recovery/ % | RSDs/% | ||
---|---|---|---|---|---|
Intra-day | Inter-day | ||||
BIF | 5 | 89.8 | 5.8 | 9.1 | |
10 | 93.1 | 6.2 | 8.6 | ||
20 | 96.7 | 4.1 | 7.5 | ||
OXY | 5 | 91.6 | 7.4 | 9.3 | |
10 | 93.5 | 3.6 | 4.2 | ||
20 | 94.5 | 2.9 | 5.8 | ||
NIT | 5 | 87.3 | 8.2 | 10.8 | |
10 | 91.4 | 6.5 | 9.3 | ||
20 | 95.7 | 4.2 | 6.7 |
Table 2 Recoveries and precisions of this method (n=3)
Analyte | Spiked/ (μg/kg) | Recovery/ % | RSDs/% | ||
---|---|---|---|---|---|
Intra-day | Inter-day | ||||
BIF | 5 | 89.8 | 5.8 | 9.1 | |
10 | 93.1 | 6.2 | 8.6 | ||
20 | 96.7 | 4.1 | 7.5 | ||
OXY | 5 | 91.6 | 7.4 | 9.3 | |
10 | 93.5 | 3.6 | 4.2 | ||
20 | 94.5 | 2.9 | 5.8 | ||
NIT | 5 | 87.3 | 8.2 | 10.8 | |
10 | 91.4 | 6.5 | 9.3 | ||
20 | 95.7 | 4.2 | 6.7 |
Sample | Analyte | Found/(μg/kg) | Recovery/% | RSD/% (n=3) |
---|---|---|---|---|
1 | BIF | N. D. | 87.6 | 6.2 |
OXY | N. D. | 90.3 | 4.1 | |
NIT | N. D. | 88.6 | 9.3 | |
2 | BIF | N. D. | 89.3 | 7.2 |
OXY | N. D. | 92.5 | 4.6 | |
NIT | N. D. | 90.4 | 5.8 | |
3 | BIF | N. D. | 91.3 | 2.9 |
OXY | N. D. | 93.7 | 3.1 | |
NIT | N. D. | 90.4 | 5.4 | |
4 | BIF | N. D. | 88.8 | 10.1 |
OXY | N. D. | 92.5 | 6.5 | |
NIT | N. D. | 91.7 | 5.7 | |
5 | BIF | N. D. | 92.6 | 1.8 |
OXY | N. D. | 89.7 | 3.5 | |
NIT | N. D. | 95.4 | 4.2 | |
6 | BIF | N. D. | 91.7 | 4.8 |
OXY | N. D. | 91.3 | 6.9 | |
NIT | N. D. | 90.2 | 10.5 | |
7 | BIF | N. D. | 90.5 | 9.1 |
OXY | N. D. | 92.5 | 5.6 | |
NIT | N. D. | 89.1 | 1.8 | |
8 | BIF | N. D. | 85.7 | 2.7 |
OXY | N. D. | 91.3 | 3.4 | |
NIT | N. D. | 88.6 | 8.3 | |
9 | BIF | N. D. | 94.5 | 6.2 |
OXY | N. D. | 92.6 | 3.0 | |
NIT | N. D. | 89.6 | 7.7 | |
10 | BIF | N. D. | 92.5 | 3.9 |
OXY | N. D. | 90.6 | 4.5 | |
NIT | N. D. | 91.3 | 11.3 |
Table 3 Analytical results and spiked recoveries for the determination of three Des in rice samples
Sample | Analyte | Found/(μg/kg) | Recovery/% | RSD/% (n=3) |
---|---|---|---|---|
1 | BIF | N. D. | 87.6 | 6.2 |
OXY | N. D. | 90.3 | 4.1 | |
NIT | N. D. | 88.6 | 9.3 | |
2 | BIF | N. D. | 89.3 | 7.2 |
OXY | N. D. | 92.5 | 4.6 | |
NIT | N. D. | 90.4 | 5.8 | |
3 | BIF | N. D. | 91.3 | 2.9 |
OXY | N. D. | 93.7 | 3.1 | |
NIT | N. D. | 90.4 | 5.4 | |
4 | BIF | N. D. | 88.8 | 10.1 |
OXY | N. D. | 92.5 | 6.5 | |
NIT | N. D. | 91.7 | 5.7 | |
5 | BIF | N. D. | 92.6 | 1.8 |
OXY | N. D. | 89.7 | 3.5 | |
NIT | N. D. | 95.4 | 4.2 | |
6 | BIF | N. D. | 91.7 | 4.8 |
OXY | N. D. | 91.3 | 6.9 | |
NIT | N. D. | 90.2 | 10.5 | |
7 | BIF | N. D. | 90.5 | 9.1 |
OXY | N. D. | 92.5 | 5.6 | |
NIT | N. D. | 89.1 | 1.8 | |
8 | BIF | N. D. | 85.7 | 2.7 |
OXY | N. D. | 91.3 | 3.4 | |
NIT | N. D. | 88.6 | 8.3 | |
9 | BIF | N. D. | 94.5 | 6.2 |
OXY | N. D. | 92.6 | 3.0 | |
NIT | N. D. | 89.6 | 7.7 | |
10 | BIF | N. D. | 92.5 | 3.9 |
OXY | N. D. | 90.6 | 4.5 | |
NIT | N. D. | 91.3 | 11.3 |
Fig. 7 Chromatograms of (a) Des standard solution, spiked rice samples (20 μg/kg) (b) direct injection and (c) pretreatment with the proposed MSPE method
Pretreatment method | Instrument | Sample | Extraction time/min | LOD/(μg/kg) | Recovery/% | Reference | ||
---|---|---|---|---|---|---|---|---|
QuEChERS | LC-MS/MS | spinach | 1 | -4 | 76- | 114 | [19] | |
DSPE | GC-MS | soil | 10 | 3.5 | -10.5 | 76- | 111 | [20] |
ASE-DLLE | GC-MS | soil | 14 | 1.2 | -2.6 | 83.5- | 103.3 | [20] |
SPE | GC-MS | rice | 25 | 70- | 107 | [21] | ||
MSPE | HPLC-UV | wheat flour | 25 | 0.24 | -0.68 | 88.8- | 96.6 | [22] |
MSPE | HPLC-UV | rice | 6 | 0.4 | -0.6 | 87.3- | 96.7 | this method |
Table 4 Comparison of the present method with the national standard method and reported methods for the determination of Des
Pretreatment method | Instrument | Sample | Extraction time/min | LOD/(μg/kg) | Recovery/% | Reference | ||
---|---|---|---|---|---|---|---|---|
QuEChERS | LC-MS/MS | spinach | 1 | -4 | 76- | 114 | [19] | |
DSPE | GC-MS | soil | 10 | 3.5 | -10.5 | 76- | 111 | [20] |
ASE-DLLE | GC-MS | soil | 14 | 1.2 | -2.6 | 83.5- | 103.3 | [20] |
SPE | GC-MS | rice | 25 | 70- | 107 | [21] | ||
MSPE | HPLC-UV | wheat flour | 25 | 0.24 | -0.68 | 88.8- | 96.6 | [22] |
MSPE | HPLC-UV | rice | 6 | 0.4 | -0.6 | 87.3- | 96.7 | this method |
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