Chinese Journal of Chromatography ›› 2023, Vol. 41 ›› Issue (3): 241-249.DOI: 10.3724/SP.J.1123.2022.06004
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WANG Jin1, YE Kaixiao1, TIAN Yan1, LIU Ke1, LIANG Liuling1, LI Qingqian1, HUANG Ning1,*(), WANG Xinting2
Received:
2022-06-15
Online:
2023-03-08
Published:
2023-03-02
Contact:
HUANG Ning, Tel:(0771)5773975,E-mail:hn_517@qq.com.
Supported by:
CLC Number:
WANG Jin, YE Kaixiao, TIAN Yan, LIU Ke, LIANG Liuling, LI Qingqian, HUANG Ning, WANG Xinting. Simultaneous determination of 22 antibiotics in environmental water samples by solid phase extraction-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2023, 41(3): 241-249.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.06004
Compound | Precursor ion (m/z) | Product ions (m/z) | Fragm- entor/V | Collision energies/eV |
---|---|---|---|---|
Lincomycin | 407.0 | 359.0, 126.0* | 140 | 30, 15 |
Penicillin G | 335.0 | 289.0, 91.0* | 160 | 23, 50 |
Marbofloxacin | 363.0 | 344.9, 72.1* | 120 | 20, 25 |
Fleroxacin | 369.9 | 326.0*, 269.0 | 140 | 15, 25 |
Ofloxacin | 361.9 | 317.9*, 260.8 | 140 | 15, 25 |
Norfloxacin | 320.0 | 302.0, 276.0* | 120 | 20, 15 |
Ciprofloxacin | 332.0 | 313.9, 288.0* | 130 | 20, 15 |
Enrofloxacin | 360.0 | 341.9, 316.0* | 130 | 20, 15 |
Orbifloxacin | 395.9 | 378.0, 352.0* | 140 | 15, 15 |
Sarafloxacin | 386.0 | 367.8, 342.0* | 140 | 20, 15 |
Difloxacin | 400.0 | 381.9, 356.0* | 140 | 20, 15 |
Sparfloxacin | 393.0 | 349.0*, 291.8 | 150 | 15, 25 |
Clindamycin | 425.0 | 377.0, 126.0* | 140 | 30, 15 |
Oleandomycin | 688.3 | 544.2, 158.0* | 150 | 30, 15 |
Tylosin | 916.8 | 772.8, 174.3* | 230 | 40, 30 |
Penicillin V | 351.0 | 256.8, 228.9* | 170 | 8, 10 |
Leucomycin A5 | 772.7 | 173.9*, 109.2 | 200 | 30, 40 |
Oxolinic acid | 261.9 | 243.9*, 216.1 | 100 | 15, 30 |
Flumequine | 261.9 | 243.9*, 202.1 | 110 | 15, 35 |
Cloxacillin | 435.9 | 220.1, 177.9* | 190 | 15, 25 |
Josamycin | 828.8 | 174.1*, 109.1 | 210 | 35, 50 |
Dicloxacillin | 470.0 | 451.9, 211.8* | 190 | 15, 25 |
Table 1 MS parameters of the target compounds
Compound | Precursor ion (m/z) | Product ions (m/z) | Fragm- entor/V | Collision energies/eV |
---|---|---|---|---|
Lincomycin | 407.0 | 359.0, 126.0* | 140 | 30, 15 |
Penicillin G | 335.0 | 289.0, 91.0* | 160 | 23, 50 |
Marbofloxacin | 363.0 | 344.9, 72.1* | 120 | 20, 25 |
Fleroxacin | 369.9 | 326.0*, 269.0 | 140 | 15, 25 |
Ofloxacin | 361.9 | 317.9*, 260.8 | 140 | 15, 25 |
Norfloxacin | 320.0 | 302.0, 276.0* | 120 | 20, 15 |
Ciprofloxacin | 332.0 | 313.9, 288.0* | 130 | 20, 15 |
Enrofloxacin | 360.0 | 341.9, 316.0* | 130 | 20, 15 |
Orbifloxacin | 395.9 | 378.0, 352.0* | 140 | 15, 15 |
Sarafloxacin | 386.0 | 367.8, 342.0* | 140 | 20, 15 |
Difloxacin | 400.0 | 381.9, 356.0* | 140 | 20, 15 |
Sparfloxacin | 393.0 | 349.0*, 291.8 | 150 | 15, 25 |
Clindamycin | 425.0 | 377.0, 126.0* | 140 | 30, 15 |
Oleandomycin | 688.3 | 544.2, 158.0* | 150 | 30, 15 |
Tylosin | 916.8 | 772.8, 174.3* | 230 | 40, 30 |
Penicillin V | 351.0 | 256.8, 228.9* | 170 | 8, 10 |
Leucomycin A5 | 772.7 | 173.9*, 109.2 | 200 | 30, 40 |
Oxolinic acid | 261.9 | 243.9*, 216.1 | 100 | 15, 30 |
Flumequine | 261.9 | 243.9*, 202.1 | 110 | 15, 35 |
Cloxacillin | 435.9 | 220.1, 177.9* | 190 | 15, 25 |
Josamycin | 828.8 | 174.1*, 109.1 | 210 | 35, 50 |
Dicloxacillin | 470.0 | 451.9, 211.8* | 190 | 15, 25 |
Compound | Regression equation | r | Linear range/ (μg/L) | MDL/ (ng/L) | LOQ/ (ng/L) | Surface water | Urban waste water | ||||||||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
25 ng/L | 100 ng/L | 250 ng/L | 25 ng/L | 100 ng/L | 250 ng/L | ||||||||||||||||||||||||||||||||
Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | ||||||||||||||||||||||||||
Lincomycin | y=2229.45x-3812.90 | 0.998 | 2-160 | 8.1 | 32.4 | 120 | 5.1 | 122 | 3.8 | 127 | 2.8 | 113 | 2.7 | 121 | 2.1 | 120 | 2.8 | ||||||||||||||||||||
Penicillin G | y=90.89x-153.76 | 0.999 | 2-160 | 9.3 | 37.2 | 111 | 8.3 | 114 | 2.3 | 102 | 5.2 | 128 | 12.2 | 126 | 2.1 | 115 | 3.4 | ||||||||||||||||||||
Marbofloxacin | y=867.25x-3960.57 | 0.995 | 5-160 | 5.7 | 22.8 | 126 | 6.1 | 94.8 | 14.0 | 97.5 | 12.6 | 95.0 | 4.1 | 83.3 | 8.5 | 79.1 | 10.5 | ||||||||||||||||||||
Fleroxacin | y=534.56x-2469.78 | 0.999 | 5-160 | 7.8 | 31.2 | 120 | 7.8 | 80.9 | 14.0 | 81.4 | 15.1 | 94.8 | 3.8 | 83.5 | 9.6 | 76.3 | 10.4 | ||||||||||||||||||||
Ofloxacin | y=319.21x-1406.60 | 0.995 | 5-160 | 7.4 | 29.6 | 132 | 6.8 | 99.7 | 15.0 | 106 | 12.7 | 51.8 | 2.1 | 68.0 | 9.9 | 73.8 | 7.4 | ||||||||||||||||||||
Norfloxacin | y=167.45x-641.00 | 0.998 | 5-100 | 10.7 | 42.8 | 116 | 11.4 | 94.1 | 20.1 | 92.7 | 21.9 | 50.1 | 1.9 | 73.2 | 11.1 | 66.6 | 10.1 | ||||||||||||||||||||
Ciprofloxacin | y=166.99x-330.58 | 0.995 | 2-100 | 8.1 | 32.4 | 157 | 2.9 | 101 | 15.3 | 114 | 6.3 | 96.5 | 5.3 | 96.9 | 11.6 | 84.7 | 9.4 | ||||||||||||||||||||
Enrofloxacin | y=799.09x-906.65 | 0.998 | 2-100 | 5.1 | 20.4 | 92.3 | 1.4 | 73.1 | 13.0 | 80.6 | 11.0 | 108 | 6.1 | 90.1 | 7.9 | 83.6 | 4.5 | ||||||||||||||||||||
Orbifloxacin | y=1083.85x-1562.31 | 0.998 | 2-100 | 7.1 | 28.4 | 121 | 4.7 | 86.5 | 2.5 | 85.1 | 4.4 | 75.1 | 9.3 | 82.9 | 2.1 | 80.1 | 3.4 | ||||||||||||||||||||
Sarafloxacin | y=369.11x-685.07 | 0.996 | 2-100 | 6.3 | 25.2 | 140 | 3.0 | 102 | 3.5 | 117 | 3.6 | 92.0 | 7.3 | 108 | 3.6 | 99.0 | 3.3 | ||||||||||||||||||||
Difloxacin | y=893.39x-492.10 | 0.996 | 2-160 | 3.9 | 15.6 | 94.3 | 3.9 | 79.5 | 7.1 | 82.1 | 3.5 | 114 | 7.4 | 110 | 3.6 | 105 | 2.5 | ||||||||||||||||||||
Sparfloxacin | y=723.65x-1003.24 | 0.997 | 2-100 | 3.8 | 15.2 | 127 | 4.3 | 94.6 | 1.9 | 96.4 | 4.9 | 62.2 | 10.6 | 82.9 | 2.4 | 79.5 | 2.6 | ||||||||||||||||||||
Clindamycin | y=2872.32x-170.75 | 0.999 | 2-160 | 5.6 | 22.4 | 102 | 1.4 | 111 | 2.1 | 115 | 1.6 | 112 | 3.1 | 119 | 2.3 | 114 | 2.0 | ||||||||||||||||||||
Oleandomycin | y=1781.20x+851.51 | 0.999 | 2-160 | 9.7 | 38.8 | 84.2 | 3.9 | 85.2 | 2.3 | 88.8 | 2.7 | 77.4 | 4.8 | 84.4 | 2.4 | 84.6 | 1.5 | ||||||||||||||||||||
Tylosin | y=413.73x-26.90 | 0.999 | 2-160 | 2.4 | 9.6 | 91.6 | 2.6 | 81.2 | 1.5 | 82.8 | 2.5 | 78.6 | 2.9 | 87.4 | 1.8 | 83.2 | 2.8 | ||||||||||||||||||||
Penicillin V | y=135.46x-97.73 | 0.999 | 2-160 | 6.1 | 24.4 | 66.5 | 11.0 | 86.7 | 5.1 | 82.0 | 3.7 | 116 | 8.0 | 82.4 | 3.3 | 72.8 | 11.1 | ||||||||||||||||||||
Leucomycin A5 | y=310.19x+1.20 | 0.999 | 2-160 | 2.9 | 11.6 | 91.0 | 4.1 | 82.4 | 1.8 | 86.0 | 2.2 | 84.1 | 3.6 | 91.3 | 1.9 | 89.1 | 3.4 | ||||||||||||||||||||
Oxolinic acid | y=3435.39x+2147.32 | 0.999 | 2-160 | 2.8 | 11.2 | 95.9 | 6.1 | 94.0 | 2.7 | 98.0 | 3.8 | 92.5 | 16.5 | 129 | 1.4 | 127 | 1.9 | ||||||||||||||||||||
Flumequine | y=895.64x+177.80 | 0.998 | 2-160 | 2.3 | 9.2 | 104 | 5.4 | 98.6 | 1.0 | 102 | 3.5 | 89.7 | 16.9 | 126 | 2.6 | 126 | 2.3 | ||||||||||||||||||||
Cloxacillin | y=264.77x-265.29 | 0.999 | 2-160 | 2.7 | 10.8 | 61.2 | 7.2 | 88.0 | 5.4 | 81.1 | 2.8 | 106 | 9.1 | 72.8 | 5.3 | 72.4 | 4.3 | ||||||||||||||||||||
Josamycin | y=550.19x+337.48 | 0.998 | 2-160 | 2.8 | 11.2 | 64.9 | 7.2 | 76.8 | 2.8 | 85.6 | 3.0 | 76.6 | 3.1 | 92.4 | 1.2 | 94.4 | 2.2 | ||||||||||||||||||||
Dicloxacillin | y=157.93x-38.90 | 0.998 | 2-160 | 3.2 | 12.8 | 84.3 | 9.1 | 73.7 | 5.9 | 76.5 | 2.3 | 110 | 9.9 | 74.0 | 7.5 | 73.6 | 2.0 |
Table 2 Regression equations, linear ranges, correlation coefficients (r), method detected limits (MDLs), LOQs, spiked recoveries (Re.) and RSDs (n=6) of the target compounds
Compound | Regression equation | r | Linear range/ (μg/L) | MDL/ (ng/L) | LOQ/ (ng/L) | Surface water | Urban waste water | ||||||||||||||||||||||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
25 ng/L | 100 ng/L | 250 ng/L | 25 ng/L | 100 ng/L | 250 ng/L | ||||||||||||||||||||||||||||||||
Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | Re./ % | RSD/ % | ||||||||||||||||||||||||||
Lincomycin | y=2229.45x-3812.90 | 0.998 | 2-160 | 8.1 | 32.4 | 120 | 5.1 | 122 | 3.8 | 127 | 2.8 | 113 | 2.7 | 121 | 2.1 | 120 | 2.8 | ||||||||||||||||||||
Penicillin G | y=90.89x-153.76 | 0.999 | 2-160 | 9.3 | 37.2 | 111 | 8.3 | 114 | 2.3 | 102 | 5.2 | 128 | 12.2 | 126 | 2.1 | 115 | 3.4 | ||||||||||||||||||||
Marbofloxacin | y=867.25x-3960.57 | 0.995 | 5-160 | 5.7 | 22.8 | 126 | 6.1 | 94.8 | 14.0 | 97.5 | 12.6 | 95.0 | 4.1 | 83.3 | 8.5 | 79.1 | 10.5 | ||||||||||||||||||||
Fleroxacin | y=534.56x-2469.78 | 0.999 | 5-160 | 7.8 | 31.2 | 120 | 7.8 | 80.9 | 14.0 | 81.4 | 15.1 | 94.8 | 3.8 | 83.5 | 9.6 | 76.3 | 10.4 | ||||||||||||||||||||
Ofloxacin | y=319.21x-1406.60 | 0.995 | 5-160 | 7.4 | 29.6 | 132 | 6.8 | 99.7 | 15.0 | 106 | 12.7 | 51.8 | 2.1 | 68.0 | 9.9 | 73.8 | 7.4 | ||||||||||||||||||||
Norfloxacin | y=167.45x-641.00 | 0.998 | 5-100 | 10.7 | 42.8 | 116 | 11.4 | 94.1 | 20.1 | 92.7 | 21.9 | 50.1 | 1.9 | 73.2 | 11.1 | 66.6 | 10.1 | ||||||||||||||||||||
Ciprofloxacin | y=166.99x-330.58 | 0.995 | 2-100 | 8.1 | 32.4 | 157 | 2.9 | 101 | 15.3 | 114 | 6.3 | 96.5 | 5.3 | 96.9 | 11.6 | 84.7 | 9.4 | ||||||||||||||||||||
Enrofloxacin | y=799.09x-906.65 | 0.998 | 2-100 | 5.1 | 20.4 | 92.3 | 1.4 | 73.1 | 13.0 | 80.6 | 11.0 | 108 | 6.1 | 90.1 | 7.9 | 83.6 | 4.5 | ||||||||||||||||||||
Orbifloxacin | y=1083.85x-1562.31 | 0.998 | 2-100 | 7.1 | 28.4 | 121 | 4.7 | 86.5 | 2.5 | 85.1 | 4.4 | 75.1 | 9.3 | 82.9 | 2.1 | 80.1 | 3.4 | ||||||||||||||||||||
Sarafloxacin | y=369.11x-685.07 | 0.996 | 2-100 | 6.3 | 25.2 | 140 | 3.0 | 102 | 3.5 | 117 | 3.6 | 92.0 | 7.3 | 108 | 3.6 | 99.0 | 3.3 | ||||||||||||||||||||
Difloxacin | y=893.39x-492.10 | 0.996 | 2-160 | 3.9 | 15.6 | 94.3 | 3.9 | 79.5 | 7.1 | 82.1 | 3.5 | 114 | 7.4 | 110 | 3.6 | 105 | 2.5 | ||||||||||||||||||||
Sparfloxacin | y=723.65x-1003.24 | 0.997 | 2-100 | 3.8 | 15.2 | 127 | 4.3 | 94.6 | 1.9 | 96.4 | 4.9 | 62.2 | 10.6 | 82.9 | 2.4 | 79.5 | 2.6 | ||||||||||||||||||||
Clindamycin | y=2872.32x-170.75 | 0.999 | 2-160 | 5.6 | 22.4 | 102 | 1.4 | 111 | 2.1 | 115 | 1.6 | 112 | 3.1 | 119 | 2.3 | 114 | 2.0 | ||||||||||||||||||||
Oleandomycin | y=1781.20x+851.51 | 0.999 | 2-160 | 9.7 | 38.8 | 84.2 | 3.9 | 85.2 | 2.3 | 88.8 | 2.7 | 77.4 | 4.8 | 84.4 | 2.4 | 84.6 | 1.5 | ||||||||||||||||||||
Tylosin | y=413.73x-26.90 | 0.999 | 2-160 | 2.4 | 9.6 | 91.6 | 2.6 | 81.2 | 1.5 | 82.8 | 2.5 | 78.6 | 2.9 | 87.4 | 1.8 | 83.2 | 2.8 | ||||||||||||||||||||
Penicillin V | y=135.46x-97.73 | 0.999 | 2-160 | 6.1 | 24.4 | 66.5 | 11.0 | 86.7 | 5.1 | 82.0 | 3.7 | 116 | 8.0 | 82.4 | 3.3 | 72.8 | 11.1 | ||||||||||||||||||||
Leucomycin A5 | y=310.19x+1.20 | 0.999 | 2-160 | 2.9 | 11.6 | 91.0 | 4.1 | 82.4 | 1.8 | 86.0 | 2.2 | 84.1 | 3.6 | 91.3 | 1.9 | 89.1 | 3.4 | ||||||||||||||||||||
Oxolinic acid | y=3435.39x+2147.32 | 0.999 | 2-160 | 2.8 | 11.2 | 95.9 | 6.1 | 94.0 | 2.7 | 98.0 | 3.8 | 92.5 | 16.5 | 129 | 1.4 | 127 | 1.9 | ||||||||||||||||||||
Flumequine | y=895.64x+177.80 | 0.998 | 2-160 | 2.3 | 9.2 | 104 | 5.4 | 98.6 | 1.0 | 102 | 3.5 | 89.7 | 16.9 | 126 | 2.6 | 126 | 2.3 | ||||||||||||||||||||
Cloxacillin | y=264.77x-265.29 | 0.999 | 2-160 | 2.7 | 10.8 | 61.2 | 7.2 | 88.0 | 5.4 | 81.1 | 2.8 | 106 | 9.1 | 72.8 | 5.3 | 72.4 | 4.3 | ||||||||||||||||||||
Josamycin | y=550.19x+337.48 | 0.998 | 2-160 | 2.8 | 11.2 | 64.9 | 7.2 | 76.8 | 2.8 | 85.6 | 3.0 | 76.6 | 3.1 | 92.4 | 1.2 | 94.4 | 2.2 | ||||||||||||||||||||
Dicloxacillin | y=157.93x-38.90 | 0.998 | 2-160 | 3.2 | 12.8 | 84.3 | 9.1 | 73.7 | 5.9 | 76.5 | 2.3 | 110 | 9.9 | 74.0 | 7.5 | 73.6 | 2.0 |
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