Chinese Journal of Chromatography ›› 2020, Vol. 38 ›› Issue (2): 232-237.DOI: 10.3724/SP.J.1123.2019.04008
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CHEN Keyun, LI Ling, JU Xiang, WANG Yanli, LIU Yanming()
Received:
2019-04-02
Online:
2020-02-08
Published:
2020-12-10
Contact:
LIU Yanming
Supported by:
CHEN Keyun, LI Ling, JU Xiang, WANG Yanli, LIU Yanming. Study and comparison of detection methods for prochloraz and its metabolite residue in garlic bolting[J]. Chinese Journal of Chromatography, 2020, 38(2): 232-237.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2019.04008
Method | Compound | Linear range/(mg/L) | Linear equation | r2 | LOD/(mg/kg) | LOQ/(mg/kg) |
y1: response of prochloraz using hydrolysis method; y2: response of prochloraz using QuEChERS method; y3: response of 2, 4, 6-trichlorophenol using QuEChERS method; x1: mass concentration (mg/L) of prochloraz using hydrolysis method; x2: mass concentration (mg/L) of prochloraz using QuEChERS method; x3: mass concentration (mg/L) of 2, 4, 6-trichlorophenol using QuEChERS method. | ||||||
Hydrolysis | prochloraz | 0.01-2 | y1=3.18×105x1-1106 | 0.9992 | 0.002 | 0.005 |
QuEChERS | prochloraz | 0.01-2 | y2=1.50×105x2-3998 | 0.9993 | 0.012 | 0.039 |
2, 4, 6-trichlorophenol | 0.01-2 | y3=7.25×105x3-9037 | 0.9993 | 0.001 | 0.003 |
Table 1 Linear equations, r2, LODs, and LOQs for prochloraz and its metabolites
Method | Compound | Linear range/(mg/L) | Linear equation | r2 | LOD/(mg/kg) | LOQ/(mg/kg) |
y1: response of prochloraz using hydrolysis method; y2: response of prochloraz using QuEChERS method; y3: response of 2, 4, 6-trichlorophenol using QuEChERS method; x1: mass concentration (mg/L) of prochloraz using hydrolysis method; x2: mass concentration (mg/L) of prochloraz using QuEChERS method; x3: mass concentration (mg/L) of 2, 4, 6-trichlorophenol using QuEChERS method. | ||||||
Hydrolysis | prochloraz | 0.01-2 | y1=3.18×105x1-1106 | 0.9992 | 0.002 | 0.005 |
QuEChERS | prochloraz | 0.01-2 | y2=1.50×105x2-3998 | 0.9993 | 0.012 | 0.039 |
2, 4, 6-trichlorophenol | 0.01-2 | y3=7.25×105x3-9037 | 0.9993 | 0.001 | 0.003 |
Method | Compound | Added/ (mg/kg) | Recovery/ % | RSD/ % |
Hydrolysis | prochloraz | 0.005 | 104.2 | 6.2 |
0.05 | 95.1 | 4.7 | ||
0.1 | 101.9 | 1.3 | ||
QuEChERS | prochloraz | 0.05 | 98.0 | 4.3 |
0.1 | 92.0 | 2.2 | ||
0.5 | 96.2 | 1.9 | ||
2, 4, 6-trichlorophenol | 0.005 | 105.4 | 6.8 | |
0.05 | 86.7 | 4.6 | ||
0.1 | 81.5 | 2.7 |
Table 2 Average spiked recoveries and RSDs of prochloraz and its metabolites (n=6)
Method | Compound | Added/ (mg/kg) | Recovery/ % | RSD/ % |
Hydrolysis | prochloraz | 0.005 | 104.2 | 6.2 |
0.05 | 95.1 | 4.7 | ||
0.1 | 101.9 | 1.3 | ||
QuEChERS | prochloraz | 0.05 | 98.0 | 4.3 |
0.1 | 92.0 | 2.2 | ||
0.5 | 96.2 | 1.9 | ||
2, 4, 6-trichlorophenol | 0.005 | 105.4 | 6.8 | |
0.05 | 86.7 | 4.6 | ||
0.1 | 81.5 | 2.7 |
Sample No. | Hydrolysis method | QuEChERS method | |||
Total amount of prochloraz/(mg/kg) | Total amount of prochloraz/(mg/kg) | Matrix of prochloraz/(mg/kg) | 2, 4, 6-Trichlorophenol/ (mg/kg) | ||
1 | 1.82 | 1.42 | 0.753 | 0.349 | |
2 | 1.23 | 0.708 | 0.649 | 0.0308 | |
3 | 1.03 | 0.634 | 0.412 | 0.116 | |
4 | 0.998 | 0.881 | 0.596 | 0.149 | |
5 | 0.851 | 0.697 | 0.374 | 0.169 | |
6 | 0.740 | 0.230 | 0.110 | 0.0628 | |
7 | 0.643 | 0.270 | 0.108 | 0.0846 | |
8 | 0.514 | 0.202 | 0.116 | 0.0449 | |
9 | 0.416 | 0.207 | 0.0983 | 0.0570 | |
10 | 0.127 | 0.0997 | 0.0445 | 0.0289 |
Table 3 Analytical results for prochloraz in garlic bolting
Sample No. | Hydrolysis method | QuEChERS method | |||
Total amount of prochloraz/(mg/kg) | Total amount of prochloraz/(mg/kg) | Matrix of prochloraz/(mg/kg) | 2, 4, 6-Trichlorophenol/ (mg/kg) | ||
1 | 1.82 | 1.42 | 0.753 | 0.349 | |
2 | 1.23 | 0.708 | 0.649 | 0.0308 | |
3 | 1.03 | 0.634 | 0.412 | 0.116 | |
4 | 0.998 | 0.881 | 0.596 | 0.149 | |
5 | 0.851 | 0.697 | 0.374 | 0.169 | |
6 | 0.740 | 0.230 | 0.110 | 0.0628 | |
7 | 0.643 | 0.270 | 0.108 | 0.0846 | |
8 | 0.514 | 0.202 | 0.116 | 0.0449 | |
9 | 0.416 | 0.207 | 0.0983 | 0.0570 | |
10 | 0.127 | 0.0997 | 0.0445 | 0.0289 |
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