Chinese Journal of Chromatography ›› 2022, Vol. 40 ›› Issue (12): 1119-1127.DOI: 10.3724/SP.J.1123.2022.05025
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XUE Gaoxu1,2, WANG Qinyi3, CAO Ling1,*(), SUN Jing1,*(), YANG Gongjun3, FENG Youlong1, FANG Fang1
Received:
2022-05-20
Online:
2022-12-08
Published:
2022-11-29
Contact:
CAO Ling, SUN Jing
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CLC Number:
XUE Gaoxu, WANG Qinyi, CAO Ling, SUN Jing, YANG Gongjun, FENG Youlong, FANG Fang. Rapid screening of 14 antibacterial drugs in anti-acne cosmetics using ion mobility spectrometry coupled with solid-phase extraction[J]. Chinese Journal of Chromatography, 2022, 40(12): 1119-1127.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2022.05025
Fig. 1 Responses of the 14 antibacterial drugs to different ion source voltages analyzed by ESI-IMS ESI-IMS: electrospray ionization-ion mobility spectrometry.
No. | Compound | Linear equation | r2 | Linear range/(mg/L) | LOD/(mg/L) |
---|---|---|---|---|---|
1 | fluconazole | y=8.23×104x-1.36×104 | 0.9997 | 5.068-81.09 | 0.30 |
2 | norfloxacin | y=1.28×105x-3.71×104 | 0.9997 | 5.092-81.46 | 0.20 |
3 | ciprofloxacin | y=9.66×104x-4.07×104 | 0.9998 | 4.208-67.32 | 0.25 |
4 | pefloxacin | y=7.08×104x-9.43×104 | 0.9993 | 3.609-57.75 | 0.50 |
5 | bifonazole | y=8.61×104x+4.64×104 | 0.9995 | 4.998-79.96 | 0.10 |
6 | sarafloxacin hydrochloride | y=1.00×105x-6.43×104 | 0.9994 | 4.340-79.35 | 0.50 |
7 | miconazole nitrate | y=1.56×105x+5.20×104 | 0.9996 | 5.078-81.25 | 0.20 |
8 | clotrimazole | y=7.34×104x-1.11×104 | 0.9996 | 5.059-80.93 | 0.15 |
9 | enoxacin | y=5.33×104x-3.24×104 | 0.9998 | 4.631-74.10 | 0.40 |
10 | naftifine hydrochloride | y=3.71×105x-9.53×102 | 0.9991 | 5.094-81.49 | 0.03 |
11 | econazole nitrate | y=1.20×105x-7.75×102 | 0.9997 | 5.077-81.23 | 0.20 |
12 | ofloxacin | y=1.95×105x-1.69×105 | 0.9995 | 5.078-81.25 | 0.13 |
13 | difloxacin hydrochloride | y=9.87×104x-7.37×104 | 0.9995 | 4.960-79.35 | 0.25 |
14 | ketoconazole | y=1.04×105x-4.82×102 | 0.9993 | 5.072-81.16 | 0.15 |
Table 1 Linear equations, linear ranges, and LODs of the 14 antibacterial drugs analyzed by HPLC
No. | Compound | Linear equation | r2 | Linear range/(mg/L) | LOD/(mg/L) |
---|---|---|---|---|---|
1 | fluconazole | y=8.23×104x-1.36×104 | 0.9997 | 5.068-81.09 | 0.30 |
2 | norfloxacin | y=1.28×105x-3.71×104 | 0.9997 | 5.092-81.46 | 0.20 |
3 | ciprofloxacin | y=9.66×104x-4.07×104 | 0.9998 | 4.208-67.32 | 0.25 |
4 | pefloxacin | y=7.08×104x-9.43×104 | 0.9993 | 3.609-57.75 | 0.50 |
5 | bifonazole | y=8.61×104x+4.64×104 | 0.9995 | 4.998-79.96 | 0.10 |
6 | sarafloxacin hydrochloride | y=1.00×105x-6.43×104 | 0.9994 | 4.340-79.35 | 0.50 |
7 | miconazole nitrate | y=1.56×105x+5.20×104 | 0.9996 | 5.078-81.25 | 0.20 |
8 | clotrimazole | y=7.34×104x-1.11×104 | 0.9996 | 5.059-80.93 | 0.15 |
9 | enoxacin | y=5.33×104x-3.24×104 | 0.9998 | 4.631-74.10 | 0.40 |
10 | naftifine hydrochloride | y=3.71×105x-9.53×102 | 0.9991 | 5.094-81.49 | 0.03 |
11 | econazole nitrate | y=1.20×105x-7.75×102 | 0.9997 | 5.077-81.23 | 0.20 |
12 | ofloxacin | y=1.95×105x-1.69×105 | 0.9995 | 5.078-81.25 | 0.13 |
13 | difloxacin hydrochloride | y=9.87×104x-7.37×104 | 0.9995 | 4.960-79.35 | 0.25 |
14 | ketoconazole | y=1.04×105x-4.82×102 | 0.9993 | 5.072-81.16 | 0.15 |
No. | Compound | Migration time/ms | K0/(cm2/(V·s)) | LOD/(mg/L) | MLOD*/(μg/g) |
---|---|---|---|---|---|
1 | fluconazole | 11.85±0.02 | 1.242±0.002 | 0.25 | 1.0 |
2 | norfloxacin | 12.48±0.03 | 1.179±0.002 | 0.25 | 1.0 |
3 | ciprofloxacin | 12.74±0.02 | 1.155±0.002 | 0.25 | 1.0 |
4 | pefloxacin | 12.83±0.02 | 1.147±0.002 | 0.25 | 1.0 |
5 | bifonazole | 13.27±0.02 | 1.108±0.002 | 0.05 | 0.2 |
6 | sarafloxacin hydrochloride | 13.71±0.03 | 1.073±0.002 | 0.25 | 1.0 |
7 | miconazole nitrate | 14.15±0.02 | 1.040±0.002 | 0.10 | 0.4 |
8 | clotrimazole | 11.46±0.02 | 1.284±0.002 | 0.05 | 0.2 |
9 | enoxacin | 12.34±0.03 | 1.192±0.003 | 0.30 | 1.2 |
10 | naftifine hydrochloride | 12.65±0.02 | 1.163±0.002 | 0.05 | 0.2 |
11 | econazole nitrate | 13.69±0.02 | 1.075±0.002 | 0.05 | 0.2 |
12 | ofloxacin | 13.86±0.02 | 1.061±0.001 | 0.25 | 1.0 |
13 | difloxacin hydrochloride | 14.12±0.02 | 1.042±0.002 | 0.20 | 0.8 |
14 | ketoconazole | 16.39±0.02 | 0.898±0.001 | 0.25 | 1.0 |
Table 2 Migration times, approximate mobilities (K0), and LODs of the 14 antibacterial drugs analyzed by ESI-IMS (n=6)
No. | Compound | Migration time/ms | K0/(cm2/(V·s)) | LOD/(mg/L) | MLOD*/(μg/g) |
---|---|---|---|---|---|
1 | fluconazole | 11.85±0.02 | 1.242±0.002 | 0.25 | 1.0 |
2 | norfloxacin | 12.48±0.03 | 1.179±0.002 | 0.25 | 1.0 |
3 | ciprofloxacin | 12.74±0.02 | 1.155±0.002 | 0.25 | 1.0 |
4 | pefloxacin | 12.83±0.02 | 1.147±0.002 | 0.25 | 1.0 |
5 | bifonazole | 13.27±0.02 | 1.108±0.002 | 0.05 | 0.2 |
6 | sarafloxacin hydrochloride | 13.71±0.03 | 1.073±0.002 | 0.25 | 1.0 |
7 | miconazole nitrate | 14.15±0.02 | 1.040±0.002 | 0.10 | 0.4 |
8 | clotrimazole | 11.46±0.02 | 1.284±0.002 | 0.05 | 0.2 |
9 | enoxacin | 12.34±0.03 | 1.192±0.003 | 0.30 | 1.2 |
10 | naftifine hydrochloride | 12.65±0.02 | 1.163±0.002 | 0.05 | 0.2 |
11 | econazole nitrate | 13.69±0.02 | 1.075±0.002 | 0.05 | 0.2 |
12 | ofloxacin | 13.86±0.02 | 1.061±0.001 | 0.25 | 1.0 |
13 | difloxacin hydrochloride | 14.12±0.02 | 1.042±0.002 | 0.20 | 0.8 |
14 | ketoconazole | 16.39±0.02 | 0.898±0.001 | 0.25 | 1.0 |
Fig. 4 IMS spectra of the 14 antibacterial drugs 1. fluconazole; 2. norfloxacin; 3. ciprofloxacin; 4. pefloxacin; 5. bifonazole; 6. sarafloxacin hydrochloride; 7. miconazole nitrate; 8. clotrimazole; 9. enoxacin; 10. naftifine hydrochloride; 11. econazole nitrate; 12. ofloxacin; 13. difloxacin hydrochloride; 14. ketoconazole.
No. | Compound | Added/ (μg/g) | Found/ (μg/g) | Recovery/ % | RSD/ % |
---|---|---|---|---|---|
1 | fluconazole | 39.92 | 35.90 | 89.9 | 1.2 |
59.88 | 51.73 | 86.4 | 1.0 | ||
79.84 | 72.94 | 91.4 | 1.0 | ||
2 | norfloxacin | 39.84 | 37.61 | 94.4 | 1.4 |
59.76 | 54.61 | 91.4 | 2.1 | ||
79.68 | 71.50 | 89.7 | 1.6 | ||
3 | ciprofloxacin | 33.24 | 29.18 | 87.8 | 2.1 |
49.86 | 44.62 | 89.5 | 6.1 | ||
66.48 | 61.28 | 92.2 | 3.8 | ||
4 | pefloxacin | 28.52 | 23.64 | 82.9 | 0.9 |
42.78 | 36.78 | 86.0 | 0.6 | ||
57.04 | 46.54 | 81.6 | 0.7 | ||
5 | bifonazole | 39.44 | 34.66 | 87.9 | 1.4 |
59.16 | 51.95 | 87.8 | 1.3 | ||
78.88 | 68.17 | 86.4 | 1.7 | ||
6 | sarafloxacin | 34.32 | 26.81 | 78.1 | 0.1 |
hydrochloride | 51.48 | 40.76 | 79.2 | 0.2 | |
68.64 | 55.91 | 81.5 | 0.2 | ||
7 | miconazole nitrate | 39.84 | 32.22 | 80.9 | 1.5 |
59.76 | 49.17 | 82.3 | 1.1 | ||
79.68 | 66.77 | 83.8 | 4.9 | ||
8 | clotrimazole | 39.80 | 34.18 | 85.9 | 0.2 |
59.70 | 53.90 | 90.3 | 0.1 | ||
79.60 | 64.61 | 81.2 | 0.1 | ||
9 | enoxacin | 36.60 | 32.34 | 88.4 | 0.6 |
54.90 | 48.06 | 87.5 | 0.6 | ||
73.20 | 59.27 | 81.0 | 0.4 | ||
10 | naftifine | 40.00 | 34.15 | 85.4 | 0.1 |
hydrochloride | 60.00 | 51.92 | 86.5 | 0.7 | |
80.00 | 64.69 | 80.9 | 0.1 | ||
11 | econazole nitrate | 39.88 | 34.05 | 85.4 | 0.1 |
59.82 | 51.26 | 85.7 | 0.8 | ||
79.76 | 64.50 | 80.9 | 0.1 | ||
12 | ofloxacin | 39.88 | 35.02 | 87.8 | 0.1 |
59.82 | 51.98 | 86.9 | 0.3 | ||
79.76 | 67.85 | 85.1 | 0.4 | ||
13 | difloxacin | 38.84 | 34.47 | 88.7 | 0.6 |
hydrochloride | 58.26 | 52.12 | 89.5 | 1.0 | |
77.68 | 66.66 | 85.8 | 0.1 | ||
14 | ketoconazole | 39.92 | 33.91 | 84.9 | 0.5 |
59.88 | 53.20 | 88.9 | 0.3 | ||
79.84 | 74.51 | 93.3 | 0.2 |
Table 3 Recoveries and precisions of the 14 antibacterial drugs in the blank sample at three spiked levels analyzed by HPLC (n=3)
No. | Compound | Added/ (μg/g) | Found/ (μg/g) | Recovery/ % | RSD/ % |
---|---|---|---|---|---|
1 | fluconazole | 39.92 | 35.90 | 89.9 | 1.2 |
59.88 | 51.73 | 86.4 | 1.0 | ||
79.84 | 72.94 | 91.4 | 1.0 | ||
2 | norfloxacin | 39.84 | 37.61 | 94.4 | 1.4 |
59.76 | 54.61 | 91.4 | 2.1 | ||
79.68 | 71.50 | 89.7 | 1.6 | ||
3 | ciprofloxacin | 33.24 | 29.18 | 87.8 | 2.1 |
49.86 | 44.62 | 89.5 | 6.1 | ||
66.48 | 61.28 | 92.2 | 3.8 | ||
4 | pefloxacin | 28.52 | 23.64 | 82.9 | 0.9 |
42.78 | 36.78 | 86.0 | 0.6 | ||
57.04 | 46.54 | 81.6 | 0.7 | ||
5 | bifonazole | 39.44 | 34.66 | 87.9 | 1.4 |
59.16 | 51.95 | 87.8 | 1.3 | ||
78.88 | 68.17 | 86.4 | 1.7 | ||
6 | sarafloxacin | 34.32 | 26.81 | 78.1 | 0.1 |
hydrochloride | 51.48 | 40.76 | 79.2 | 0.2 | |
68.64 | 55.91 | 81.5 | 0.2 | ||
7 | miconazole nitrate | 39.84 | 32.22 | 80.9 | 1.5 |
59.76 | 49.17 | 82.3 | 1.1 | ||
79.68 | 66.77 | 83.8 | 4.9 | ||
8 | clotrimazole | 39.80 | 34.18 | 85.9 | 0.2 |
59.70 | 53.90 | 90.3 | 0.1 | ||
79.60 | 64.61 | 81.2 | 0.1 | ||
9 | enoxacin | 36.60 | 32.34 | 88.4 | 0.6 |
54.90 | 48.06 | 87.5 | 0.6 | ||
73.20 | 59.27 | 81.0 | 0.4 | ||
10 | naftifine | 40.00 | 34.15 | 85.4 | 0.1 |
hydrochloride | 60.00 | 51.92 | 86.5 | 0.7 | |
80.00 | 64.69 | 80.9 | 0.1 | ||
11 | econazole nitrate | 39.88 | 34.05 | 85.4 | 0.1 |
59.82 | 51.26 | 85.7 | 0.8 | ||
79.76 | 64.50 | 80.9 | 0.1 | ||
12 | ofloxacin | 39.88 | 35.02 | 87.8 | 0.1 |
59.82 | 51.98 | 86.9 | 0.3 | ||
79.76 | 67.85 | 85.1 | 0.4 | ||
13 | difloxacin | 38.84 | 34.47 | 88.7 | 0.6 |
hydrochloride | 58.26 | 52.12 | 89.5 | 1.0 | |
77.68 | 66.66 | 85.8 | 0.1 | ||
14 | ketoconazole | 39.92 | 33.91 | 84.9 | 0.5 |
59.88 | 53.20 | 88.9 | 0.3 | ||
79.84 | 74.51 | 93.3 | 0.2 |
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