嘧菌酯在杨梅中的残留行为及膳食暴露风险评估

doi:10.3969/j.issn.1004-1524.2023.04.21

浙江农业学报 ›› 2023, Vol. 35 ›› Issue (4): 942-951.DOI: 10.3969/j.issn.1004-1524.2023.04.21

嘧菌酯在杨梅中的残留行为及膳食暴露风险评估

张春荣(), 郭钤, 孔丽萍, 吴园园, 林琴, 许振岚, 赵学平, 汤涛()

浙江省农业科学院农产品质量安全与营养研究所,农产品质量安全危害因子与风险防控国家重点实验室,农业农村部农药残留检测重点实验室,浙江杭州 310021

收稿日期:2021-12-31 出版日期:2023-04-25 发布日期:2023-05-05
作者简介:张春荣(1970—),女,河南温县人,硕士,副研究员,研究方向为农药风险评估。E-mail:crzhang001@126.com
通讯作者: ^*汤涛,E-mail:tangtao80@126.com
基金资助:
国家自然科学基金(31501668)

Residue behavior and dietary exposure risk assessment of azoxystrobin in waxberry

ZHANG Chunrong(), GUO Qian, KONG Liping, WU Yuanyuan, LIN Qin, XU Zhenlan, ZHAO Xueping, TANG Tao()

State Key Laboratory for Managing Biotic and Chemical Threats to the Quality and Safety of Agro-Products, Key Laboratory for Pesticide Residue Detection of Ministry of Agriculture and Rural Affairs, Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2021-12-31 Online:2023-04-25 Published:2023-05-05

摘要/Abstract

摘要：

建立嘧菌酯在杨梅中的残留分析方法,考察嘧菌酯在杨梅中的储藏稳定性,通过开展50%嘧菌酯水分散粒剂在杨梅树上1年(2018年)6地的田间试验,明确嘧菌酯在杨梅上的残留特征及膳食风险。杨梅样品中嘧菌酯经乙腈提取,碱性氧化铝净化,超高效液相色谱-串联质谱(UPLC-MS/MS)检测,外标法定量。结果表明,在 0.001~0.05 mg·L^-1 范围内,嘧菌酯在溶剂及基质中的峰面积与其对应的质量浓度间线性关系均良好,R²≥0.999 1。当添加质量分数为0.01~30.0 mg·kg^-1时,嘧菌酯在杨梅中添加回收率为90%~98%,相对标准偏差(RSD)为1.8%~7.9%,定量限(LOQ)为0.01 mg·kg^-1,该方法能用于检测嘧菌酯在杨梅中的残留量。杨梅中嘧菌酯在冷冻储藏条件下较为稳定,在≤-18 ℃储藏条件下杨梅样品储藏650 d,其降解率低于14.3%。田间试验结果表明,嘧菌酯在杨梅上降解较快,其消解符合一级动力学方程,半衰期为2.2~5.0 d。按照300 mg·kg^-1 (制剂用药量:1 667倍液)对杨梅树施用50%嘧菌酯水分散粒剂2次,施药间隔10 d,最后一次施药后20、25、30 d,杨梅中嘧菌酯的残留量分别为0.012~0.57、<0.010~0.52、<0.010~0.28 mg·kg^-1。嘧菌酯的普通人群国家估算每日摄入量(national estimated daily intake,NEDI)是6.111 4 mg,风险商(risk quotient,RQ)为48.5%,对一般人群健康风险较低。

关键词: 嘧菌酯, 杨梅, 残留, 消解, 储藏稳定性, 膳食风险评估

Abstract:

In order to clarify the residual characteristic and dietary risk of azoxystrobin in waxberry, an analytical method was developed for the determination of azoxystrobin residues in waxberry by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and the storage stability of azoxystrobin in waxberry was also investigated. The field trials of 50% water dispersible granule of azoxystrobin were conducted in six provinces in the year of 2018. The samples were extracted by acetonitrile, purified by alkaline alumina and quantified by external standard method. The results showed that the calibration curve with good linearity was obtained in the concentration range from 0.001 to 0.05 mg·L^-1, with correlation coefficients (R²) not less than 0.999 1. At the spiked levels of 0.01 to 30.0 mg·kg^-1, the average recovery of azoxystrobin in waxberry was 90%-98% with relative standard deviations (RSD) of 1.8%-7.9%. The limit of quantitation (LOQ) of azoxystrobin in waxberry matrix was 0.01 mg·kg^-1. The degradation rates of azoxystrobin in waxberry samples with initial concentration of 5 mg·kg^-1 were lower than 14.3% at no more than -18℃, indicating that azoxystrobin can be steadily stored for at least 650 days in waxberry samples. The dissipation dynamics of azoxystrobin was fitted to the first-order kinetics equation, and the half-lives of azoxystrobin in waxberry were 2.2-5.0 d, indicating azoxystrobin was an easily degradable pesticide (T_1/2<30 d). 50% azoxystrobin water dispersible granule was sprayed twice with an interval of 10 d at the recommended high dosage (300 mg·kg^-1) in the waxberry. The final residues of azoxystrobin in the waxberry were 0.012-0.57,<0.010-0.52,<0.010-0.28 mg·kg^-1 at day 20, 25 and 30 after application, respectively, which were lower than the maximum residue limits of azoxystrobin in berry and other small fruits. The long-term dietary intake risk assessment indicated that the national estimated daily intake (NEDI) of azoxystrobin was 6.111 4 mg, with a risk quotient (RQ) of 48.5%. The results showed that the residual levels of azoxystrobin in waxberry did not pose unacceptable risks to the general population.

Key words: azoxystrobin, waxberry, residue, dissipation, storage stability, dietary risk assessment

中图分类号:

S667.6

张春荣, 郭钤, 孔丽萍, 吴园园, 林琴, 许振岚, 赵学平, 汤涛. 嘧菌酯在杨梅中的残留行为及膳食暴露风险评估[J]. 浙江农业学报, 2023, 35(4): 942-951.

ZHANG Chunrong, GUO Qian, KONG Liping, WU Yuanyuan, LIN Qin, XU Zhenlan, ZHAO Xueping, TANG Tao. Residue behavior and dietary exposure risk assessment of azoxystrobin in waxberry[J]. Acta Agriculturae Zhejiangensis, 2023, 35(4): 942-951.

图/表 8

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地点Site	项目Item	品种Variety	树高Height of tree/m
浙江兰溪Lanxi, Zhejiang	最终残留量/消解Final residue/Dissipation	东魁Dongkui	4.0
贵州贵阳Guiyang, Guizhou	最终残留量/消解Final residue/Dissipation	荸荠Biqi	2.3
湖南张家界Zhangjiajie, Hunan	最终残留量/消解Final residue/Dissipation	乌梅Wumei	3.0
云南玉溪Yuxi, Yunnan	最终残留量Final residue	冬葵Dongkui	3.0~3.2
安徽安庆Anqing, Anhui	最终残留量Final residue	黑炭梅Heitanmei	3.0
福建福安Fu’an, Fujian	最终残留量Final residue	东魁Dongkui	2.0~2.5

地点Site	项目Item	品种Variety	树高Height of tree/m
浙江兰溪Lanxi, Zhejiang	最终残留量/消解Final residue/Dissipation	东魁Dongkui	4.0
贵州贵阳Guiyang, Guizhou	最终残留量/消解Final residue/Dissipation	荸荠Biqi	2.3
湖南张家界Zhangjiajie, Hunan	最终残留量/消解Final residue/Dissipation	乌梅Wumei	3.0
云南玉溪Yuxi, Yunnan	最终残留量Final residue	冬葵Dongkui	3.0~3.2
安徽安庆Anqing, Anhui	最终残留量Final residue	黑炭梅Heitanmei	3.0
福建福安Fu’an, Fujian	最终残留量Final residue	东魁Dongkui	2.0~2.5

储藏时间 Time/d	储藏样品残留量 Residual amount of the stored analytical sample/(mg·kg^-1)			降解率 Degradation rate/%	质控样品回收率 Recovery of the quality control sample/%			相对标准偏差 RSD/%
储藏时间 Time/d	1	2	平均Average	降解率 Degradation rate/%	1	2	平均Average	相对标准偏差 RSD/%
0	4.6	5.1	4.9	—	97	103	100	4.4
182	4.5	4.8	4.7	4.1	92	94	93	1.9
390	4.7	4.4	4.6	6.1	86	93	89	5.6
540	4.6	4.6	4.6	6.1	83	91	87	6.8
650	3.8	4.5	4.2	14.3	77	89	83	10.6

储藏时间 Time/d	储藏样品残留量 Residual amount of the stored analytical sample/(mg·kg^-1)			降解率 Degradation rate/%	质控样品回收率 Recovery of the quality control sample/%			相对标准偏差 RSD/%
储藏时间 Time/d	1	2	平均Average	降解率 Degradation rate/%	1	2	平均Average	相对标准偏差 RSD/%
0	4.6	5.1	4.9	—	97	103	100	4.4
182	4.5	4.8	4.7	4.1	92	94	93	1.9
390	4.7	4.4	4.6	6.1	86	93	89	5.6
540	4.6	4.6	4.6	6.1	83	91	87	6.8
650	3.8	4.5	4.2	14.3	77	89	83	10.6

试验地点 Site	消解方程 Dynamic equation	原始沉积量 Initial concentration/(mg·kg^-1)	相关系数 r	半衰期 Half-life/d
浙江兰溪Lanxi,Zhejiang	C_t=7.6602e^-0.1705t	23.4	0.909 8	4.1
湖南张家界Zhangjiajie,Hunan	C_t=6.5679e^-0.1376t	9.3	0.984 9	5.0
贵州贵阳Guiyang,Guizhou	C_t=3.4054e^-0.3126t	4.7	0.938 2	2.2

嘧菌酯在杨梅中的残留行为及膳食暴露风险评估

Residue behavior and dietary exposure risk assessment of azoxystrobin in waxberry

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添加水平 Spiked level/(mg·kg^-1)	回收率Recovery						相对标准偏差 RSD
添加水平 Spiked level/(mg·kg^-1)	1	2	3	4	5	平均值Average	相对标准偏差 RSD
0.01	95	95	95	85	80	90	7.9
0.5	94	92	90	90	92	92	1.8
30	95	98	97	99	102	98	2.6

采收间隔期 Interval to harvest/d	最终残留量 Terminal residue	残留试验中值 STMR	最高残留值 HR
20	0.012、0.017、0.032、0.039、0.21、0.28、0.29、0.30、0.33、0.34、0.38、0.57	0.28	0.57
25	<0.010、<0.010、0.11、0.14、0.15、0.16、0.17、0.19、0.21、0.28、0.47、0.52	0.16	0.52
30	<0.010、<0.010、<0.010、0.077、0.085、0.11、0.14、0.15、0.17、	0.12	0.28
	0.23、0.25、0.28

食物种类 Food groups	膳食量 Food intake/kg	参考限量或残留中值 Reference maximum residue limits or STMR	限量来源 Source of maximum residue limits	国家估计每日摄入量 NEDI/mg	日允许摄入量 Acceptable daily intake/mg	风险商 Risk quotient /%
米及其制品Rice and their products	0.239 9	1	中国China	0.239 900	ADI×63
面及其制品Flour and their products	0.138 5	1.5	中国China	0.207 750
其他谷类Other grains	0.023 3	1	中国China	0.023 300
薯类Potato	0.049 5	0.2	中国China	0.009 900
干豆类及其制品Dried beans and their products	0.016 0	0.5	中国China	0.008 000
深色蔬菜Dark colored vegetables	0.091 5	10	中国China	0.915 000
浅色蔬菜Light colored vegetables	0.183 7	20	中国China	3.674 000
腌制蔬菜Pickled vegetables	0.010 3	—	—	—
水果Fruits	0.045 7	0.28	残留中值STMR	0.012 800
坚果Nuts	0.003 9	1	中国China	0.003 900
畜禽类Livestock and poultry class	0.079 5	0.07^*	中国China	0.005 565
奶及其制品Milk and their products	0.026 3	0.01^*	中国China	0.000 263
蛋及其制品Egg and their products	0.023 6	0.01^*	中国China	0.000 236
鱼虾类Fish and shrimp	0.030 1	—	—	—
植物油Vegetable oil	0.032 7	0.5	中国China	0.016 350
动物油Animal fat	0.008 7	—	—	—
糖、淀粉Sugar, starch	0.004 4	1	中国China	0.004 400
食盐Salt	0.012 0	30	中国China	0.360 000
酱油Soy sauce	0.009 0	70	中国China	0.630 000
合计Total	1.028 6			6.111 400	12.6	48.5

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