2012 14 1 67-73 Chinese Journal of Pesticide Science http / /www. nyxxb. com. cn * 310058 - GC-ECD - V V = 7 1 m m m = 5 3 0. 15 - GC-ECD 1 0. 5 0. 01 mg /kg 82. 1% ~ 97. 8% 90. 9% ~ 92. 0% RSD 1. 6% ~ 6. 2% 1. 6% ~ 3. 1% LOD S /N = 3 0. 06 ng LOQ 0. 01 mg /kg 2010 0. 1 mg /kg RQ DOI 10. 3969 /j. issn. 1008-7303. 2012. 01. 10 O657. 71 X836 A 1008-7303 2012 01-0067-07 De te rmination of azoxystrobin re sidue in Panax ginseng and Panax quinquefolium and die tary intake risk assessment WU Jialun * WANG Huaichang WU Xiuting ZHAO Jing YANG Na'na Ministry of Agriculture Key Laboratory of Molecular Biology of Crop Pathogens and Insects Institute of Pesticide and Environmental Toxicology Zhejiang University Hangzhou 310058 China Abstract A method for the determination of azoxystrobin residues in Panax ginseng and Panax quinquefolium was described. The residues were extracted with acetonitrile-water V acetonitrile V water = 7 1 assisted by ultrasonic cleaned up with florisil-neutral alumina-activated charcoal 5 3 0. 15 m m m mixed column and dichloromethane by means of liquid-liquid partition. Quantitative analysis was performed with gas chromatography equipped with ECD electronic capture detector. The fortified recoveries and relative standard deviation RSD were 82. 1% - 97. 8% and 1. 6% - 6. 2% in Panax ginseng 90. 9% - 92. 0% and 1. 6% - 3. 1% in Panax quinquefolium at three spiked levels 1 0. 5 and 0. 01 mg /kg. The limit of detection S /N = 3 was 0. 06 ng and the limit of quantification LOQ of the detection method was 0. 01 mg /kg. The method was applied to monitor the residue status of azoxystrobin in some representative Panax ginseng and Panax quinquefolium planting areas 2011-10-13 2011-11-21. * Author for correspondence E-mail jlwu@ zju. edu. cn.
68 Vol. 14 and make risk assessment in 2010. The result of the study show ed that the maximum residue in the sample was 0. 1 mg /kg. By calculating risk quotient RQ was very low and the residue could be declined to the safe level. Key words azoxystrobin Panax ginseng Panax quinquefolium pesticide residue risk assessment azoxystrobin 99. 0% Dr. Ehrenstorfer Celite 545 1 3 150 ~ 250 μm 75 ~ 150 μm 0. 45 μm azoxystrobin 600 4 h 130 2 h 4 9 3% b c1 5% 1 h ATP 600 10 11 2 h 105 4 h GPC MSPD SPE 12 14 4 GAP 15 25% GAP MRL 1. 2 0. 5 mg /L 1. 2. 1 1. 2. 1. 1 2010 MRL 16 17 4 9 24 1 - GC-ECD 1. 2. 1. 2 4. 00 g 0. 01 g 250 ml 1 g 70 ml MRL 10 ml 30 min 1 h 1 1. 1 20 830 μm - 20 40 ml 1. 2. 1. 3 2 cm 9 cm - m Agilent GC-7890A 63 Ni-ECD m m = 5 3 Agilent DD01 0. 15 2 cm 30 ml Sartorius V V = 1 9 0. 01 g 80 ml
No. 1 69 5 ml 250 ml 40 ml 10% dose mg /kg CRL calculated residue 30 ml 1 min 3 1 ml 2 ml0. 45 μm GC-ECD bw body weight kg RQ risk quotient ADI acceptable daily 1. 2. 2 GC-ECD KB-5 18 30 m 0. 32 mm 0. 25 μm 320 250 2 min 20 /min 230 3 min 25 /min 280 15 min 1 ml /min 30 ml /min 13 15 3 ml /min 1 μl - - 60 ml /min 1. 2. 3 88 ± 0. 101 0 g 0. 000 1 g 2. 31 % 1 000 mg /L 10 ml 100 ml 100 mg /L - 2 5 Bertuzzi 19-1 0. 5 0. 1 0. 05 0. 01 mg /L - V 1. 2. 2 1 μl V = 7 1 94 ± 3 4. 22 % 2. 2 1. 2. 4 1 0. 5 0. 01 mg /L 3 12 6 1. 2. 1 1. 2. 2 NPD Chistensen 13 RSD 1. 3 14 SPE 1 2 18 EED = CRL FI /bw RQ = EED /ADI 1 2 EED estimated exposure level mg /kg FI food intake kg intake mg / kg bw RQ > 1 RQ < 1 2 160 1 min 30 /min 190 2. 1 Sorbent 6 mg /L 20 - - - GPC 1 1 Table 1 Comparison of different means of purify Recovery /% 1 2 3 Average recovery /% RSD /% Florisil 90. 8 88. 8 87. 7 89. 1 1. 7 Neutral alumina 85. 9 82. 4 83. 8 84. 1 2. 1 Activated charcoal 10. 3 12. 1 11. 2 11. 2 7. 8 m m m = 5 3 0. 15 m florisil m neutral alumina m activated charcoal = 5 3 0. 15 88. 3 93. 9 92. 6 91. 6 2. 9
70 Vol. 14 - m m m = 5 3 0. 15 2. 3 1 0. 01 ~ 5. 0 mg /L Fig. 1 Standard calibration curve for azoxystrobin mass conc. from 0. 01 to 5. 0 mg /L 2. 5 2-82. 1% ~ 97. 8% RSD 1. 6% ~ V V = 1 9 6. 2% 90. 9% ~ 92. 0% RSD 1. 6% ~ 3. 1% 2. 4 LOQ 0. 01 mg /kg LOD S /N = 3 0. 06 ng 84. 5% ~ 103. 2% RSD 1. 3% ~ 2. 0% y x 1 2 Table 2 2 Recoveries of azoxystrobin in Panax ginseng and Panax quinquefolium Samples Spiked level / mg /kg Recovery /% 1 2 3 Average recovery /% RSD /% Panax ginseng 1. 00 101. 3 107. 9 95. 4 97. 6 91. 3 93. 3 97. 8 6. 2 0. 50 89. 3 90. 4 90. 7 90. 3 1. 6 88. 3 91. 0 92. 1 0. 01 82. 3 81. 8 79. 7 82. 1 1. 6 83. 1 83. 4 82. 0 Panax quinquefolium 1. 00 87. 3 91. 5 93. 1 94. 6 89. 9 94. 5 91. 9 3. 1 0. 50 92. 6 93. 4 90. 2 92. 0 1. 6 90. 1 93. 2 92. 4 0. 01 91. 5 94. 0 91. 1 90. 9 1. 9 89. 5 89. 7 90. 0 2. 6 40. 0% 2010 4 24 0. 1 mg /L 3 2 1 MRL 4 GB 26130 2010 MRL 0. 5 mg /L 45. 0% 30. 0% 5. 0 mg /L 0. 5 mg /L 3 2 MRL 60. 0%
No. 1 71 A. B. 0. 5 mg /kg C. D. 0. 5 mg /kg E. A. Standard chromatogram of azoxystrobin B. Panax ginseng sample fortified with azoxystrobin 0. 5 mg /kg C. Blank sample of Panax ginseng D. Panax quinquefolium sample fortified with azoxystrobin 0. 5 mg /kg E. Blank sample of Panax quinquefolium 2 Fig. 2 GC chromatogram of azoxystrobin JMPR 2008 RQ ADI 0 ~ 0. 2 mg / kg bw 20 2008 2 8 21 2002-2005 8 60 kg MRL 0. 000 57 kg 15 2008-2009 3 2 25% 3. 5 ~ 4. 7 d LD 50 > 5 000 mg /kg LD 50 > 2 000 mg /kg 5 2010 7 d
72 Vol. 14 Table 3 Samples Panax ginseng 3 n = 6 2010 Azoxystrobin residues in Panax ginseng and Panax quinquefolium n = 6 2010 Place Residue / mg /kg Ji'an City Jilin Province 0. 065 ± 0. 002 0. 042 ± 0. 004 0. 100 ± 0. 003 0. 068 ± 0. 003 Baishan City Jinlin Province 0. 070 ± 0. 001 Tonghua Count Jilin Province 0. 060 ± 0. 001 0. 063 ± 0. 003 0. 050 ± 0. 002 Fusong Count Jilin Province 0. 052 ± 0. 010 Zhejiang Chinese Medical University 0. 019 ± 0. 003 Liaoning Institute for Food and Drug Control 0. 030 ± 0. 007 0. 022 ± 0. 010 Lonquan Twon Beijing Panax quinquefolium * Not detected Huadian City Jilin Province Baishan City Jilin Province 0. 079 ± 0. 003 0. 061 ± 0. 005 0. 078 ± 0. 036 0. 088 ± 0. 025 0. 070 ± 0. 007 0. 066 ± 0. 002 Lonquan Twon Beijing 0. 080 ± 0. 007 0. 074 ± 0. 003 Zhejiang Chinese Medical University Liaoning Institute for Food and Drug Control Table 4 4 M RL of azoxystrobin in different countries MRL Country China Korea Brazil Canada Agrotype MRL / mg /kg Cucumber 0. 5 Grape 5. 0 Lychee 0. 5 Liquorice 0. 05 Angelica 0. 1 Astragalus 0. 1 Panax 0. 5 Aubergine 0. 05 Cottonseed 0. 1 Cherry 0. 4 2008 MRL Reference MRL China Pharmacy 2008 2010 1. J. 2004 15 7 444-445. DONG Lili LI Ye. Speeding up the perfection of quality standards of traditional Chinese medicine decoction pieces J. China Pharmacy 2004 15 7 444-445. in Chinese 2. J. 2008 36 23 10147-10151. GAO Qian HUA Rimao TANG Feng et al. Research status of the pesticide residue in Chinese herbal medicine J. J Anhui Agric Sci 2008 36 23 10147-10151. in Chinese 3. J. 19 3 236-238. WEI Jian LIU Yong WANG Rui. Quality problem and quality control of decoction pieces of traditional Chinese drugs J. 19 3 236-238. in Chinese 4. J. 2009 48 12 899-901. HAN Bo WU Huiming ZHU Guonian et al. Degradation of
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