Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (12): 1324-1330.DOI: 10.3724/SP.J.1123.2021.01028
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LIU Xin1,2, SUN Xiulan1,*(), CAO Jin2,*()
Received:
2021-01-25
Online:
2021-12-08
Published:
2021-05-31
Contact:
SUN Xiulan,CAO Jin
Supported by:
CLC Number:
LIU Xin, SUN Xiulan, CAO Jin. Simultaneous determination of eight carbamate pesticide residues in tomato, rice, and cabbage by online solid phase extraction/purification-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(12): 1324-1330.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.01028
Step | Time/min | φ(A)/% | φ(B)/% | Position | Function |
---|---|---|---|---|---|
1 | 0.5 | 90 | 10 | A | injection |
2 | 0.5 | 90 | 10 | B | loading |
3 | 3.0 | 90 | 10 | B | rinse |
4 | 2.0 | 35 | 65 | B | elution |
5 | 2.0 | 10 | 90 | B | elution |
6 | 2.0 | 90 | 10 | A | balance |
Table 1 Gradient conditions of online solid phase extraction/purification
Step | Time/min | φ(A)/% | φ(B)/% | Position | Function |
---|---|---|---|---|---|
1 | 0.5 | 90 | 10 | A | injection |
2 | 0.5 | 90 | 10 | B | loading |
3 | 3.0 | 90 | 10 | B | rinse |
4 | 2.0 | 35 | 65 | B | elution |
5 | 2.0 | 10 | 90 | B | elution |
6 | 2.0 | 90 | 10 | A | balance |
Compound | Retention time/min | Parent ion (m/z) | Daughter ion (m/z) | DP/ V | CE/ eV |
---|---|---|---|---|---|
Methomyl | 3.78 | 163.1 | 106.1 | 85 | 18 |
88.1* | 85 | 18 | |||
Pirimicarb | 3.90 | 239.1 | 182.2* | 85 | 20 |
72.2 | 85 | 20 | |||
Metolcarb | 5.74 | 166.1 | 109.1* | 85 | 15 |
94.0 | 85 | 40 | |||
Propoxur | 5.98 | 210.3 | 168.1 | 90 | 8 |
111.2* | 80 | 22 | |||
Carbaryl | 6.14 | 202.2 | 145.1* | 85 | 25 |
127.1 | 85 | 38 | |||
Isoprocarb | 6.33 | 194.3 | 137.2 | 50 | 15 |
95.2* | 85 | 20 | |||
Methiocarb | 6.54 | 226.1 | 169.2 | 80 | 15 |
121.2* | 80 | 25 | |||
Fenobucarb | 6.55 | 208.1 | 152.1 | 80 | 8 |
95.0* | 85 | 25 |
Table 2 Retention times and MS parameters of the eight carbamate pesticides
Compound | Retention time/min | Parent ion (m/z) | Daughter ion (m/z) | DP/ V | CE/ eV |
---|---|---|---|---|---|
Methomyl | 3.78 | 163.1 | 106.1 | 85 | 18 |
88.1* | 85 | 18 | |||
Pirimicarb | 3.90 | 239.1 | 182.2* | 85 | 20 |
72.2 | 85 | 20 | |||
Metolcarb | 5.74 | 166.1 | 109.1* | 85 | 15 |
94.0 | 85 | 40 | |||
Propoxur | 5.98 | 210.3 | 168.1 | 90 | 8 |
111.2* | 80 | 22 | |||
Carbaryl | 6.14 | 202.2 | 145.1* | 85 | 25 |
127.1 | 85 | 38 | |||
Isoprocarb | 6.33 | 194.3 | 137.2 | 50 | 15 |
95.2* | 85 | 20 | |||
Methiocarb | 6.54 | 226.1 | 169.2 | 80 | 15 |
121.2* | 80 | 25 | |||
Fenobucarb | 6.55 | 208.1 | 152.1 | 80 | 8 |
95.0* | 85 | 25 |
Compound | Linear equation | Linear range/(ng/mL) | r | LOD/(ng/mL) | LOQ/(ng/mL) |
---|---|---|---|---|---|
Methomyl | y=1.08×104x+2.51×103 | 0.5-50 | 0.9953 | 0.05 | 0.15 |
Pirimicarb | y=3.64×105x+5.03×103 | 0.1-100 | 0.9951 | 0.01 | 0.05 |
Metolcarb | y=3.63×104x+4.15×102 | 0.1-100 | 0.9991 | 0.04 | 0.10 |
Propoxur | y=2.60×104x+4.76×103 | 0.5-100 | 0.9970 | 0.05 | 0.15 |
Carbaryl | y=9.40×103x+1.87×103 | 1.0-100 | 0.9992 | 0.30 | 1.0 |
Isoprocarb | y=1.17×105x+1.11×104 | 0.1-100 | 0.9984 | 0.03 | 0.10 |
Methiocarb | y=9.29×104x+3.03×103 | 0.5-100 | 0.9970 | 0.05 | 0.20 |
Fenobucarb | y=1.74×105x+1.64×104 | 0.5-100 | 0.9979 | 0.06 | 0.20 |
Table 3 Linear equations, linear ranges, correlation coefficients (r), LODs and LOQs of the eight carbamate pesticides
Compound | Linear equation | Linear range/(ng/mL) | r | LOD/(ng/mL) | LOQ/(ng/mL) |
---|---|---|---|---|---|
Methomyl | y=1.08×104x+2.51×103 | 0.5-50 | 0.9953 | 0.05 | 0.15 |
Pirimicarb | y=3.64×105x+5.03×103 | 0.1-100 | 0.9951 | 0.01 | 0.05 |
Metolcarb | y=3.63×104x+4.15×102 | 0.1-100 | 0.9991 | 0.04 | 0.10 |
Propoxur | y=2.60×104x+4.76×103 | 0.5-100 | 0.9970 | 0.05 | 0.15 |
Carbaryl | y=9.40×103x+1.87×103 | 1.0-100 | 0.9992 | 0.30 | 1.0 |
Isoprocarb | y=1.17×105x+1.11×104 | 0.1-100 | 0.9984 | 0.03 | 0.10 |
Methiocarb | y=9.29×104x+3.03×103 | 0.5-100 | 0.9970 | 0.05 | 0.20 |
Fenobucarb | y=1.74×105x+1.64×104 | 0.5-100 | 0.9979 | 0.06 | 0.20 |
Compound | Spiked level/ (ng/mL) | Tomato | Rice | Cabbage | |||||
---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||
Methomyl | 2 | 80.40 | 5.88 | 106.81 | 3.58 | 108.59 | 5.11 | ||
10 | 86.07 | 5.77 | 94.41 | 8.92 | 93.79 | 11.92 | |||
20 | 75.98 | 8.65 | 85.87 | 10.55 | 75.32 | 6.51 | |||
Pirimicarb | 2 | 80.03 | 4.37 | 102.35 | 1.79 | 107.36 | 8.59 | ||
10 | 84.36 | 2.42 | 97.79 | 7.82 | 100.06 | 4.34 | |||
20 | 83.19 | 4.47 | 111.76 | 4.67 | 88.67 | 6.18 | |||
Metolcarb | 2 | 95.84 | 3.89 | 92.38 | 1.28 | 101.92 | 2.27 | ||
10 | 94.50 | 2.31 | 101.28 | 11.95 | 95.33 | 2.64 | |||
20 | 88.50 | 3.51 | 97.35 | 2.96 | 85.97 | 3.56 | |||
Propoxur | 2 | 77.37 | 9.99 | 82.49 | 4.56 | 101.33 | 8.19 | ||
10 | 78.89 | 5.60 | 96.52 | 7.05 | 94.95 | 6.06 | |||
20 | 111.62 | 4.98 | 90.41 | 7.26 | 84.01 | 13.14 | |||
Carbaryl | 2 | 74.98 | 8.13 | 87.72 | 7.00 | 86.09 | 5.19 | ||
10 | 82.35 | 3.84 | 94.04 | 6.80 | 89.69 | 9.74 | |||
20 | 73.76 | 9.05 | 92.17 | 3.21 | 81.22 | 7.60 | |||
Isoprocarb | 2 | 112.32 | 3.94 | 86.96 | 3.13 | 105.35 | 3.90 | ||
10 | 103.45 | 1.41 | 82.35 | 4.59 | 109.01 | 4.73 | |||
20 | 92.81 | 2.54 | 89.34 | 2.92 | 101.06 | 3.11 | |||
Methiocarb | 2 | 82.65 | 4.36 | 82.77 | 3.24 | 97.41 | 2.45 | ||
10 | 84.61 | 1.92 | 91.08 | 7.81 | 84.50 | 5.45 | |||
20 | 75.35 | 3.51 | 82.61 | 4.68 | 93.92 | 5.50 | |||
Fenobucarb | 2 | 94.84 | 2.94 | 100.63 | 1.91 | 101.28 | 3.57 | ||
10 | 97.10 | 2.24 | 103.01 | 2.99 | 98.58 | 5.23 | |||
20 | 91.03 | 3.71 | 95.72 | 2.71 | 97.01 | 4.65 |
Table 4 Recoveries and RSDs of the eight carbamate pesticides spiked in three matrices (n=6)
Compound | Spiked level/ (ng/mL) | Tomato | Rice | Cabbage | |||||
---|---|---|---|---|---|---|---|---|---|
Recovery/% | RSD/% | Recovery/% | RSD/% | Recovery/% | RSD/% | ||||
Methomyl | 2 | 80.40 | 5.88 | 106.81 | 3.58 | 108.59 | 5.11 | ||
10 | 86.07 | 5.77 | 94.41 | 8.92 | 93.79 | 11.92 | |||
20 | 75.98 | 8.65 | 85.87 | 10.55 | 75.32 | 6.51 | |||
Pirimicarb | 2 | 80.03 | 4.37 | 102.35 | 1.79 | 107.36 | 8.59 | ||
10 | 84.36 | 2.42 | 97.79 | 7.82 | 100.06 | 4.34 | |||
20 | 83.19 | 4.47 | 111.76 | 4.67 | 88.67 | 6.18 | |||
Metolcarb | 2 | 95.84 | 3.89 | 92.38 | 1.28 | 101.92 | 2.27 | ||
10 | 94.50 | 2.31 | 101.28 | 11.95 | 95.33 | 2.64 | |||
20 | 88.50 | 3.51 | 97.35 | 2.96 | 85.97 | 3.56 | |||
Propoxur | 2 | 77.37 | 9.99 | 82.49 | 4.56 | 101.33 | 8.19 | ||
10 | 78.89 | 5.60 | 96.52 | 7.05 | 94.95 | 6.06 | |||
20 | 111.62 | 4.98 | 90.41 | 7.26 | 84.01 | 13.14 | |||
Carbaryl | 2 | 74.98 | 8.13 | 87.72 | 7.00 | 86.09 | 5.19 | ||
10 | 82.35 | 3.84 | 94.04 | 6.80 | 89.69 | 9.74 | |||
20 | 73.76 | 9.05 | 92.17 | 3.21 | 81.22 | 7.60 | |||
Isoprocarb | 2 | 112.32 | 3.94 | 86.96 | 3.13 | 105.35 | 3.90 | ||
10 | 103.45 | 1.41 | 82.35 | 4.59 | 109.01 | 4.73 | |||
20 | 92.81 | 2.54 | 89.34 | 2.92 | 101.06 | 3.11 | |||
Methiocarb | 2 | 82.65 | 4.36 | 82.77 | 3.24 | 97.41 | 2.45 | ||
10 | 84.61 | 1.92 | 91.08 | 7.81 | 84.50 | 5.45 | |||
20 | 75.35 | 3.51 | 82.61 | 4.68 | 93.92 | 5.50 | |||
Fenobucarb | 2 | 94.84 | 2.94 | 100.63 | 1.91 | 101.28 | 3.57 | ||
10 | 97.10 | 2.24 | 103.01 | 2.99 | 98.58 | 5.23 | |||
20 | 91.03 | 3.71 | 95.72 | 2.71 | 97.01 | 4.65 |
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