Chinese Journal of Chromatography ›› 2021, Vol. 39 ›› Issue (4): 444-452.DOI: 10.3724/SP.J.1123.2020.08017
• Technical Notes • Previous Articles
SUN Lingli1, LIU Jia1, GUO Xiujie3, WU Lidong4, DUAN Zhengchao1, WANG Chaoran2,3,*(), WANG Lianzhi1,*()
Received:
2020-08-19
Online:
2021-04-08
Published:
2021-03-08
Contact:
WANG Chaoran,WANG Lianzhi
Supported by:
CLC Number:
SUN Lingli, LIU Jia, GUO Xiujie, WU Lidong, DUAN Zhengchao, WANG Chaoran, WANG Lianzhi. Hydrophilic interaction liquid chromatography for removal of pesticide residues in ginseng extracts[J]. Chinese Journal of Chromatography, 2021, 39(4): 444-452.
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URL: https://www.chrom-china.com/EN/10.3724/SP.J.1123.2020.08017
Fig. 1 Chromatograms of seven pesticide residues and total ginsenosides on RPLC and HILIC columns Mobile phase A: ethanol; mobile phase B: water. Elution program for C18YE (250 mm×4. 6 mm, 10 μm): 0-12 min, 0%A; 12-13 min, 0%A-60%A; 13-28 min, 60%A; 28-29 min, 60%A-90%A; 29-40 min, 90%A. Elution program for Click XIon (250 mm×4. 6 mm, 5 μm): 0-12 min, 95%A; 12-13 min, 95%A-60%A; 13-21 min, 60%A; 21-22 min, 60%A-40%A; 22-28 min, 40%A. Peak identifications: 1, 2, 3. ginsenosides; 4. carbendazim; 5. azoxystrobin; 6. procymidone; 7. iprodione; 8. propiconazole; 9. pentachloroaniline; 10. quintozene.
Fig. 3 Chromatograms of different fractions during the investigation of the maximum sample loading mass Mobile phase A: acetonitrile; mobile phase B: water. Elution program for Click XIon (250 mm×4. 6 mm, 5 μm): 0-20 min, 90%A-60%A. a. stock solutionⅠ; b. flow-through solution Ⅰ; c. flow-through solution Ⅱ; d. flow-through solution Ⅲ; e. flow-through solution Ⅳ; f. wash solution; g. eluent Ⅰ; h. eluent Ⅱ. Peak identifications: 1. Rg1; 2. Rf; 3. Re; 4. Rd; 5. Rc; 6. Rb2; 7. Rb1.
Fig. 4 Chromatograms of different fractions during the investigation of washing solution volume Mobile phase A: acetonitrile; mobile phase B: water. Elution program for Click XIon (250 mm×4. 6 mm, 5 μm): 0~20 min, 90%A~60%A. a. stock solution Ⅱ; b. flow-through solution; c. wash solution Ⅰ; d. wash solution Ⅱ; e. wash solution Ⅲ; f. wash solution Ⅳ; g. eluentⅠ; h. eluent Ⅱ. Peak identifications: 1, 2. pesticide residues; 3. Rg1; 4. Rf; 5. Re; 6. Rd; 7. Rc; 8. Rb2; 9. Rb1.
Fig. 5 Chromatograms of different fractions during the optimization of loading volume Mobile phase A: acetonitrile; mobile phase B: water. Elution program for Click XIon (250 mm×4. 6 mm, 5 μm): 0-20 min, 90%A-60%A. a. stock solution Ⅲ; b. flow-through solution; c. wash solution; d. eluentⅠ; e. eluent Ⅱ. Peak identifications: 1. pesticide residues; 2. Rg1; 3. Rf; 4. Re; 5. Rd; 6. Rc; 7. Rb2; 8. Rb1.
Fraction/ min | Category | Volume/ mL | Ginsenosides | ||
---|---|---|---|---|---|
Peak area | Percentage/ % | Purity/ % | |||
0-10 | flow-through | 600 | 1319 | 0.02 | - |
solution | |||||
10-20 | wash solution | 600 | 531596 | 7.22 | - |
20-30 | eluent Ⅰ | 600 | 1627184 | 22.10 | - |
30-45 | eluent Ⅱ | 900 | 3565080 | 72.63 | - |
45-55 | eluent Ⅲ | 600 | 2734 | 0.04 | - |
- | stock solution | 600 | 7362825 | - | 59.87 |
- | combined | 1500 | 2945130 | 94.4 | 69.61 |
solution |
Table 1 Peak area percentage of total ginsenosides in each fraction and the purity of the finished product
Fraction/ min | Category | Volume/ mL | Ginsenosides | ||
---|---|---|---|---|---|
Peak area | Percentage/ % | Purity/ % | |||
0-10 | flow-through | 600 | 1319 | 0.02 | - |
solution | |||||
10-20 | wash solution | 600 | 531596 | 7.22 | - |
20-30 | eluent Ⅰ | 600 | 1627184 | 22.10 | - |
30-45 | eluent Ⅱ | 900 | 3565080 | 72.63 | - |
45-55 | eluent Ⅲ | 600 | 2734 | 0.04 | - |
- | stock solution | 600 | 7362825 | - | 59.87 |
- | combined | 1500 | 2945130 | 94.4 | 69.61 |
solution |
No. | Retention time / min | Analyte | Contents/(mg/kg) | |
---|---|---|---|---|
Before removal | After removal | |||
1 | 11.67 | fenobucarb (仲丁威) | 0.141 | 0.03 |
2 | 12.81 | phorate (甲拌磷) | 0.116 | 0.02 |
3 | 13.13 | atraton (阿特拉通) | 0.137 | - |
4 | 13.36 | carbofuran (克百威) | 0.663 | - |
5 | 14.17 | pyrimethanil (嘧霉胺) | 0.184 | - |
6 | 15.43 | chlorpyrifos-methyl | 2.113 | - |
(甲基毒死蜱) | ||||
7 | 15.88 | ronnel (皮蝇磷) | 0.513 | - |
8 | 16.28 | ethofumesate (乙氧呋草黄) | 0.199 | 0.03 |
9 | 17.13 | isocarbophos (水胺硫磷) | 0.103 | - |
10 | 18.53 | procymidone (腐霉利) | 0.360 | - |
11 | 19.11 | tetrachlorvinphos (杀虫畏) | 0.316 | - |
12 | 19.73 | isoprothiolane (稻瘟灵) | 0.114 | 0.03 |
13 | 22.70/ | propiconazole (丙环唑) | 0.164 | - |
22.87 | ||||
14 | 24.48 | phosmet (亚胺硫磷) | 0.233 | 0.04 |
Table 2 Comparison of pesticide contents before and after the removal of 14 pesticide residues in refined samples with contents of 0.1 mg/kg and above
No. | Retention time / min | Analyte | Contents/(mg/kg) | |
---|---|---|---|---|
Before removal | After removal | |||
1 | 11.67 | fenobucarb (仲丁威) | 0.141 | 0.03 |
2 | 12.81 | phorate (甲拌磷) | 0.116 | 0.02 |
3 | 13.13 | atraton (阿特拉通) | 0.137 | - |
4 | 13.36 | carbofuran (克百威) | 0.663 | - |
5 | 14.17 | pyrimethanil (嘧霉胺) | 0.184 | - |
6 | 15.43 | chlorpyrifos-methyl | 2.113 | - |
(甲基毒死蜱) | ||||
7 | 15.88 | ronnel (皮蝇磷) | 0.513 | - |
8 | 16.28 | ethofumesate (乙氧呋草黄) | 0.199 | 0.03 |
9 | 17.13 | isocarbophos (水胺硫磷) | 0.103 | - |
10 | 18.53 | procymidone (腐霉利) | 0.360 | - |
11 | 19.11 | tetrachlorvinphos (杀虫畏) | 0.316 | - |
12 | 19.73 | isoprothiolane (稻瘟灵) | 0.114 | 0.03 |
13 | 22.70/ | propiconazole (丙环唑) | 0.164 | - |
22.87 | ||||
14 | 24.48 | phosmet (亚胺硫磷) | 0.233 | 0.04 |
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