De te rmination of azoxystrobin re sidue in Panax ginseng and Panax quinquefolium and die tary intake risk assessment

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Άγνη Κασιδιάρης
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1 Chinese Journal of Pesticide Science http / /www. nyxxb. com. cn * GC-ECD - V V = 7 1 m m m = GC-ECD mg /kg 82. 1% ~ 97. 8% 90. 9% ~ 92. 0% RSD 1. 6% ~ 6. 2% 1. 6% ~ 3. 1% LOD S /N = ng LOQ mg /kg mg /kg RQ DOI /j. issn O X836 A 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 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 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% % and 1. 6% % in Panax ginseng 90. 9% % and 1. 6% % in Panax quinquefolium at three spiked levels and mg /kg. The limit of detection S /N = 3 was ng and the limit of quantification LOQ of the detection method was mg /kg. The method was applied to monitor the residue status of azoxystrobin in some representative Panax ginseng and Panax quinquefolium planting areas * Author for correspondence jlwu@ zju. edu. cn.

2 68 Vol. 14 and make risk assessment in 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 ~ 250 μm 75 ~ 150 μm μm azoxystrobin h h 4 9 3% b c1 5% 1 h ATP h h GPC MSPD SPE GAP 15 25% GAP MRL mg /L MRL GC-ECD g g 250 ml 1 g 70 ml MRL 10 ml 30 min 1 h μm ml cm 9 cm - m Agilent GC-7890A 63 Ni-ECD m m = 5 3 Agilent DD cm 30 ml Sartorius V V = g 80 ml

3 No 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 GC-ECD KB m mm μm min 20 /min min 25 /min min 1 ml /min 30 ml /min ml /min 1 μl ml /min ± g g % mg /L 10 ml 100 ml 100 mg /L Bertuzzi mg /L - V μl V = ± % mg /L NPD Chistensen 13 RSD SPE 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 < min 30 /min Sorbent 6 mg /L GPC 1 1 Table 1 Comparison of different means of purify Recovery /% Average recovery /% RSD /% Florisil Neutral alumina Activated charcoal m m m = m florisil m neutral alumina m activated charcoal =

4 70 Vol m m m = ~ 5. 0 mg /L Fig. 1 Standard calibration curve for azoxystrobin mass conc. from to 5. 0 mg /L % ~ 97. 8% RSD 1. 6% ~ V V = % 90. 9% ~ 92. 0% RSD 1. 6% ~ 3. 1% 2. 4 LOQ mg /kg LOD S /N = ng 84. 5% ~ % 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 /% Average recovery /% RSD /% Panax ginseng Panax quinquefolium % mg /L MRL 4 GB MRL 0. 5 mg /L 45. 0% 30. 0% 5. 0 mg /L 0. 5 mg /L 3 2 MRL 60. 0%

5 No A. B mg /kg C. D 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 kg MRL kg % 3. 5 ~ 4. 7 d LD 50 > mg /kg LD 50 > mg /kg d

6 72 Vol. 14 Table 3 Samples Panax ginseng 3 n = Azoxystrobin residues in Panax ginseng and Panax quinquefolium n = Place Residue / mg /kg Ji'an City Jilin Province ± ± ± ± Baishan City Jinlin Province ± Tonghua Count Jilin Province ± ± ± Fusong Count Jilin Province ± Zhejiang Chinese Medical University ± Liaoning Institute for Food and Drug Control ± ± Lonquan Twon Beijing Panax quinquefolium * Not detected Huadian City Jilin Province Baishan City Jilin Province ± ± ± ± ± ± Lonquan Twon Beijing ± ± 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 Angelica 0. 1 Astragalus 0. 1 Panax 0. 5 Aubergine Cottonseed 0. 1 Cherry MRL Reference MRL China Pharmacy J DONG Lili LI Ye. Speeding up the perfection of quality standards of traditional Chinese medicine decoction pieces J. China Pharmacy in Chinese 2. J GAO Qian HUA Rimao TANG Feng et al. Research status of the pesticide residue in Chinese herbal medicine J. J Anhui Agric Sci in Chinese 3. J WEI Jian LIU Yong WANG Rui. Quality problem and quality control of decoction pieces of traditional Chinese drugs J in Chinese 4. J HAN Bo WU Huiming ZHU Guonian et al. Degradation of

7 No azoxystrobin residue in orange and soil J. Agrochemicals in Chinese 5. J LIU Changling GUAN Aiying ZHANG Mingxing. Azoxystrobin a broad spectrum fungicide J. World Pesticides in Chinese 6 FENOLL J RUIZ E FLORES P et al. Strobilurin residue levels in greenhouse-grown pepper and under cold-storage conditions J. J Sci Food Agric ANKE T OBERWINKLER F STEGLICH W et al. The strobilurins new antifungal antibiotics from the basidiomycete Strobilurus tenacellus J. J Antibiot CLOUGH J M GODFREY C R A GODWIN J R et al. Azoxystrobin a novel broad-spectrum systemic fungicide J. Pestic Outlook AMMERMANN E LORENZ G SCHELBERGER B et al. BAS 490 F a broad-spectrum fungicide with a new mode of action J. Proc Br Crop Prot Conf Pests Dis BARTLETT D W CLOUGH J M GODWIN J R et al. The Institute of Quality Standards and Testing Technology for Agrostrobilurin fungicides J. Pestc Manage Sci Products Chinese Academy of Agricultural Science. Risk 662. Assessment for Quality and Safety of Agro-Food Principles 11. Monilinia Methodologies and Application M. Beijing People s Medical fructicola J Publishing House in Chinese BERTUZZI P KAMPS L MILES C et al. Extraction of FANG Yali LIU Peng GUO Liyun. Sensitivity of Monilinia chlorinated pesticide residues from nonfatty samples of low fructicola isolates to azoxystrobin J. J Fruit Sci in Chinese moisture content J. J Ass Offic Anal Chem JMPR ADI ArfD J J SONG Wencheng. JMPR ADI and ArfD assessment list of BO Haibo SUN Jie. Determination of azoxystrobin residue in cauliflower and garden pea by gas chromatography J. Chin J Anal Lab in Chinese 13 CHRISTENSEN H GRANBY K. Method validation for strobilurin fungicides in cereals and fruit J. Food Addit Contam health food J. Chin J Public Health J in Chinese 20. YIN Fengping LU Zhixin LIN Mingzhen. Determination of azoxystrobin residue in cucumber and soil by GC J. Pestic Sci Adm in Chinese 15 J WANG Siwei HOU Zhiguang ZOU Jing et al. Residual decline of azoxystrobin 25% SC in ginseng environment J. Agrochemicals in Chinese 16 Commission Regulation EC No 822 /2009 S /OL http eur-lex. europa. eu /LexUriServ /LexUriServ. do uri = OJ L EN PDF / 56 /EC S /OL http eur-lex. europa. eu /LexUriServ / site /en /oj / 2007 /l _ 243 /l _ en pdf Commission Directive 2007 /56 /EC S /OL http / /eur-lex. europa. eu / LexUriServ /site /en /oj /2007 /l_243 / l_ en pdf 18. M pesticides J Pestic Sci Adm in Chinese 21. J YANG Dajin WANG Zhutian SONG Shufeng et al. Analysis study on standards for food additives in Chinese herbal medicine

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