Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (11): 1213-1221.DOI: 10.3724/SP.J.1123.2021.01029
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DAI Wei*(), LI Qiao, ZHU Ming, LIANG Yixin, CAI Qiu, WANG Mian, LI Jie, LIU Kangshu, WANG Xingning
Received:
2021-01-19
Online:
2021-11-08
Published:
2021-06-02
Contact:
DAI Wei
Supported by:
CLC Number:
DAI Wei, LI Qiao, ZHU Ming, LIANG Yixin, CAI Qiu, WANG Mian, LI Jie, LIU Kangshu, WANG Xingning. Determination of plant growth regulators in animal-derived foods using QuEChERS-isotope-labeled internal standards with high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2021, 39(11): 1213-1221.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2021.01029
Analyte | Products | China[ | EU[ | Japan[ | Australia[ |
---|---|---|---|---|---|
Chlormequat | mammals (muscle) | 0.2* | 0.3 | 0.2 | 0.2 |
chloride | mammals (liver) | 0.1* | 1.5 | 0.1 | 0.5 |
poultry (muscle) | 0.04* | 0.05 | 0.04 | 0.05 | |
eggs | 0.1* | 0.15 | 0.1 | 0.1 | |
milk | 0.5* | 0.5 | 0.5 | 0.5 | |
Thidiazuron | mammals (muscle) | - | 0.01 | 0.1 | 0.05 |
mammals (liver) | - | 0.01 | 0.1 | 0.05 | |
poultry (muscle) | - | 0.01 | 0.2 | - | |
eggs | - | 0.01 | 0.1 | - | |
milk | - | 0.01 | 0.03 | 0.01 | |
Paclobutrazol | mammals (muscle) | - | 0.01 | 0.01 | - |
mammals (liver) | - | 0.01 | 0.01 | - | |
Poultry (muscle) | - | 0.01 | 0.01 | - | |
eggs | - | 0.01 | 0.01 | - | |
milk | - | 0.01 | 0.01 | - |
Table 1 Maximum residue limits (MRLs) of the three plant growth regulators in different countries
Analyte | Products | China[ | EU[ | Japan[ | Australia[ |
---|---|---|---|---|---|
Chlormequat | mammals (muscle) | 0.2* | 0.3 | 0.2 | 0.2 |
chloride | mammals (liver) | 0.1* | 1.5 | 0.1 | 0.5 |
poultry (muscle) | 0.04* | 0.05 | 0.04 | 0.05 | |
eggs | 0.1* | 0.15 | 0.1 | 0.1 | |
milk | 0.5* | 0.5 | 0.5 | 0.5 | |
Thidiazuron | mammals (muscle) | - | 0.01 | 0.1 | 0.05 |
mammals (liver) | - | 0.01 | 0.1 | 0.05 | |
poultry (muscle) | - | 0.01 | 0.2 | - | |
eggs | - | 0.01 | 0.1 | - | |
milk | - | 0.01 | 0.03 | 0.01 | |
Paclobutrazol | mammals (muscle) | - | 0.01 | 0.01 | - |
mammals (liver) | - | 0.01 | 0.01 | - | |
Poultry (muscle) | - | 0.01 | 0.01 | - | |
eggs | - | 0.01 | 0.01 | - | |
milk | - | 0.01 | 0.01 | - |
Analyte | ESI | Parent ion (m/z) | Product ion (m/z) | Collisiom energy/eV | Fragmentor/V |
---|---|---|---|---|---|
Chlormequat cation | + | 122.1 | 58.1* | 35 | 100 |
63.0 | 35 | ||||
Thidiazuron | - | 219 | 70.9 | 35 | 80 |
100.0* | 15 | ||||
Paclobutrazol | + | 294.1 | 57.2 | 15 | 100 |
70.0* | 20 | ||||
124.9 | 25 | ||||
Chlormequat-D9 cation | + | 131 | 66.1* | 35 | 100 |
68.2 | 25 | ||||
Thidiazuron-13C6 | - | 225 | 71.1 | 35 | 100 |
100.1* | 15 | ||||
Paclobutrazol-15N3 | + | 297.0 | 73.1* | 25 | 120 |
125.0 | 25 |
Table 2 MS/MS parameters for the three plant growth regulators and their internal standards
Analyte | ESI | Parent ion (m/z) | Product ion (m/z) | Collisiom energy/eV | Fragmentor/V |
---|---|---|---|---|---|
Chlormequat cation | + | 122.1 | 58.1* | 35 | 100 |
63.0 | 35 | ||||
Thidiazuron | - | 219 | 70.9 | 35 | 80 |
100.0* | 15 | ||||
Paclobutrazol | + | 294.1 | 57.2 | 15 | 100 |
70.0* | 20 | ||||
124.9 | 25 | ||||
Chlormequat-D9 cation | + | 131 | 66.1* | 35 | 100 |
68.2 | 25 | ||||
Thidiazuron-13C6 | - | 225 | 71.1 | 35 | 100 |
100.1* | 15 | ||||
Paclobutrazol-15N3 | + | 297.0 | 73.1* | 25 | 120 |
125.0 | 25 |
Fig. 3 Effects of different dehydrating agents and clean-up agents on average recoveries of three plant growth regulators (n=3) Dehydrating agents: Method 1, 1 g NaCl+4 g MgSO4; Method 2, 1.5 g HOAc+6 g MgSO4; Method 3, 1 g NaCl+1 g C6H5Na3O7·2H2O+0.5 g C6H6Na2O7·1.5 H2O+4 g MgSO4.
Analyte | Sample | Linear range/(μg/L) | Linear equation | r2 | Matrix effect | LOD/(μg/kg) | LOQ/(μg/kg) | |
---|---|---|---|---|---|---|---|---|
Chlormequat cation | pork | 0.1-50 | y=1.91x | 0.9978 | 1.245 | 0.05 | 1.0 | |
beef | 0.1-50 | y=1.76x | 0.9975 | 1.123 | 0.05 | 0.5 | ||
chicken | 0.1-50 | y=1.79x | 0.9985 | 0.987 | 0.05 | 0.5 | ||
pork liver | 0.1-100 | y=2.01x | 0.9993 | 1.038 | 0.05 | 1.0 | ||
egg | 0.1-100 | y=1.89x | 0.9992 | 1.244 | 0.05 | 0.5 | ||
milk | 0.05-5 | y=1.13x+0.0479 | 0.9978 | 1.138 | 0.01 | 0.5 | ||
Thidiazuron | pork | 0.1-50 | y=3.71x-0.0561 | 0.9998 | 1.081 | 0.1 | 0.5 | |
beef | 0.1-50 | y=3.29x+0.0434 | 0.9999 | 1.016 | 0.1 | 1.0 | ||
chicken | 0.1-50 | y=3.49x+0.0230 | 0.9985 | 0.931 | 0.1 | 1.0 | ||
pork liver | 0.1-100 | y=2.55x+0.0229 | 0.9997 | 0.871 | 0.1 | 5.0 | ||
egg | 0.1-100 | y=4.41x-0.0511 | 0.9998 | 1.276 | 0.1 | 0.5 | ||
milk | 0.05-10 | y=3.91x+0.00738 | 0.9965 | 1.053 | 0.05 | 0.5 | ||
Paclobutrazol | pork | 0.1-50 | y=1.32x-0.00552 | 0.9987 | 0.491 | 0.05 | 0.5 | |
beef | 0.1-50 | y=1.33x-0.00968 | 0.9999 | 0.380 | 0.05 | 0.5 | ||
chicken | 0.1-50 | y=1.36x-0.00930 | 0.9985 | 0.366 | 0.05 | 0.5 | ||
pork liver | 0.1-100 | y=1.62x-0.0215 | 0.9995 | 0.257 | 0.05 | 0.5 | ||
egg | 0.1-100 | y=1.61x-0.0135 | 0.9996 | 0.363 | 0.05 | 0.5 | ||
milk | 0.05-10 | y=1.66x | 0.9997 | 0.990 | 0.01 | 0.5 |
Table 3 Linear relationships, matrix effects, LODs, and LOQs of the three plant growth regulators in different matrices
Analyte | Sample | Linear range/(μg/L) | Linear equation | r2 | Matrix effect | LOD/(μg/kg) | LOQ/(μg/kg) | |
---|---|---|---|---|---|---|---|---|
Chlormequat cation | pork | 0.1-50 | y=1.91x | 0.9978 | 1.245 | 0.05 | 1.0 | |
beef | 0.1-50 | y=1.76x | 0.9975 | 1.123 | 0.05 | 0.5 | ||
chicken | 0.1-50 | y=1.79x | 0.9985 | 0.987 | 0.05 | 0.5 | ||
pork liver | 0.1-100 | y=2.01x | 0.9993 | 1.038 | 0.05 | 1.0 | ||
egg | 0.1-100 | y=1.89x | 0.9992 | 1.244 | 0.05 | 0.5 | ||
milk | 0.05-5 | y=1.13x+0.0479 | 0.9978 | 1.138 | 0.01 | 0.5 | ||
Thidiazuron | pork | 0.1-50 | y=3.71x-0.0561 | 0.9998 | 1.081 | 0.1 | 0.5 | |
beef | 0.1-50 | y=3.29x+0.0434 | 0.9999 | 1.016 | 0.1 | 1.0 | ||
chicken | 0.1-50 | y=3.49x+0.0230 | 0.9985 | 0.931 | 0.1 | 1.0 | ||
pork liver | 0.1-100 | y=2.55x+0.0229 | 0.9997 | 0.871 | 0.1 | 5.0 | ||
egg | 0.1-100 | y=4.41x-0.0511 | 0.9998 | 1.276 | 0.1 | 0.5 | ||
milk | 0.05-10 | y=3.91x+0.00738 | 0.9965 | 1.053 | 0.05 | 0.5 | ||
Paclobutrazol | pork | 0.1-50 | y=1.32x-0.00552 | 0.9987 | 0.491 | 0.05 | 0.5 | |
beef | 0.1-50 | y=1.33x-0.00968 | 0.9999 | 0.380 | 0.05 | 0.5 | ||
chicken | 0.1-50 | y=1.36x-0.00930 | 0.9985 | 0.366 | 0.05 | 0.5 | ||
pork liver | 0.1-100 | y=1.62x-0.0215 | 0.9995 | 0.257 | 0.05 | 0.5 | ||
egg | 0.1-100 | y=1.61x-0.0135 | 0.9996 | 0.363 | 0.05 | 0.5 | ||
milk | 0.05-10 | y=1.66x | 0.9997 | 0.990 | 0.01 | 0.5 |
Matrix | Chlormequat chloride | Thidiazuron | Paclobutrazol | ||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Added/(μg/kg) | Recovery/% | RSD/% | Added/(μg/kg) | Recovery/% | RSD/% | Added/(μg/kg) | Recovery/% | RSD/% | |||||||
Pork | 1 | 75.8 | 2.6 | 0.5 | 115.8 | 3.0 | 0.5 | 86.5 | 8.2 | ||||||
2 | 84.3 | 3.6 | 1 | 89.2 | 4.2 | 1 | 107.2 | 4.4 | |||||||
10 | 94.5 | 2.5 | 5 | 104.8 | 3.5 | 5 | 102.1 | 5.5 | |||||||
Beef | 0.5 | 78.9 | 3.4 | 1 | 74.8 | 6.4 | 0.5 | 77.2 | 4.4 | ||||||
1 | 85.4 | 1.8 | 2 | 98.7 | 6.2 | 1 | 103.6 | 2.7 | |||||||
5 | 81.9 | 1.9 | 10 | 102.3 | 12.1 | 5 | 92.2 | 2.3 | |||||||
Chicken | 0.5 | 76.1 | 3.6 | 1 | 77.6 | 6.5 | 0.5 | 117.4 | 1.6 | ||||||
1 | 92.6 | 2.0 | 2 | 87.3 | 4.1 | 1 | 98.6 | 6.8 | |||||||
5 | 89.6 | 1.5 | 10 | 91.6 | 3.6 | 5 | 89.5 | 1.8 | |||||||
Pork liver | 1 | 84.3 | 2.8 | 5 | 75.3 | 4.4 | 0.5 | 115.3 | 16.1 | ||||||
2 | 80.7 | 3.2 | 10 | 78.1 | 3.9 | 1 | 95.5 | 5.4 | |||||||
10 | 76.1 | 1.9 | 50 | 70.0 | 15.2 | 5 | 70.6 | 5.2 | |||||||
Egg | 0.5 | 99.6 | 2.9 | 0.5 | 79.6 | 4.1 | 0.5 | 110.7 | 3.3 | ||||||
1 | 85.9 | 3.4 | 1 | 106.5 | 6.8 | 1 | 100.4 | 3.4 | |||||||
5 | 85.1 | 0.8 | 5 | 84.6 | 3.6 | 5 | 76.4 | 1.7 | |||||||
Milk | 0.5 | 71.3 | 7.1 | 0.5 | 92.9 | 9.8 | 0.5 | 86.0 | 6.8 | ||||||
1 | 91.2 | 7.0 | 1 | 90.1 | 4.7 | 1 | 91.6 | 3.0 | |||||||
5 | 109.8 | 10.0 | 5 | 78.7 | 12.2 | 5 | 74.7 | 13.9 |
Table 4 Spiked recoveries and RSDs of the three plant growth regulators in different matrices (n=6)
Matrix | Chlormequat chloride | Thidiazuron | Paclobutrazol | ||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Added/(μg/kg) | Recovery/% | RSD/% | Added/(μg/kg) | Recovery/% | RSD/% | Added/(μg/kg) | Recovery/% | RSD/% | |||||||
Pork | 1 | 75.8 | 2.6 | 0.5 | 115.8 | 3.0 | 0.5 | 86.5 | 8.2 | ||||||
2 | 84.3 | 3.6 | 1 | 89.2 | 4.2 | 1 | 107.2 | 4.4 | |||||||
10 | 94.5 | 2.5 | 5 | 104.8 | 3.5 | 5 | 102.1 | 5.5 | |||||||
Beef | 0.5 | 78.9 | 3.4 | 1 | 74.8 | 6.4 | 0.5 | 77.2 | 4.4 | ||||||
1 | 85.4 | 1.8 | 2 | 98.7 | 6.2 | 1 | 103.6 | 2.7 | |||||||
5 | 81.9 | 1.9 | 10 | 102.3 | 12.1 | 5 | 92.2 | 2.3 | |||||||
Chicken | 0.5 | 76.1 | 3.6 | 1 | 77.6 | 6.5 | 0.5 | 117.4 | 1.6 | ||||||
1 | 92.6 | 2.0 | 2 | 87.3 | 4.1 | 1 | 98.6 | 6.8 | |||||||
5 | 89.6 | 1.5 | 10 | 91.6 | 3.6 | 5 | 89.5 | 1.8 | |||||||
Pork liver | 1 | 84.3 | 2.8 | 5 | 75.3 | 4.4 | 0.5 | 115.3 | 16.1 | ||||||
2 | 80.7 | 3.2 | 10 | 78.1 | 3.9 | 1 | 95.5 | 5.4 | |||||||
10 | 76.1 | 1.9 | 50 | 70.0 | 15.2 | 5 | 70.6 | 5.2 | |||||||
Egg | 0.5 | 99.6 | 2.9 | 0.5 | 79.6 | 4.1 | 0.5 | 110.7 | 3.3 | ||||||
1 | 85.9 | 3.4 | 1 | 106.5 | 6.8 | 1 | 100.4 | 3.4 | |||||||
5 | 85.1 | 0.8 | 5 | 84.6 | 3.6 | 5 | 76.4 | 1.7 | |||||||
Milk | 0.5 | 71.3 | 7.1 | 0.5 | 92.9 | 9.8 | 0.5 | 86.0 | 6.8 | ||||||
1 | 91.2 | 7.0 | 1 | 90.1 | 4.7 | 1 | 91.6 | 3.0 | |||||||
5 | 109.8 | 10.0 | 5 | 78.7 | 12.2 | 5 | 74.7 | 13.9 |
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