丁氟螨酯及其代谢物对大型溞的毒性效应

doi:10.3969/j.issn.1004-1524.2022.03.16

浙江农业学报 ›› 2022, Vol. 34 ›› Issue (3): 557-565.DOI: 10.3969/j.issn.1004-1524.2022.03.16

丁氟螨酯及其代谢物对大型溞的毒性效应

安雪花¹(), 李冬雪¹, 代德茂², 余世锋², 赵美芹³, 吴声敢¹, 赵学平¹^,^*()

1.浙江省农业科学院农产品质量安全与营养研究所,浙江杭州 310021
2.北京大农时代农药技术研究所,北京 100016
3.北京科发伟业技术有限公司,北京 100125

收稿日期:2021-05-08 出版日期:2022-03-25 发布日期:2022-03-30
通讯作者: 赵学平
作者简介:*赵学平,E-mail: zhaoxp@mail.zaas.ac.cn
安雪花(1976—),女,吉林龙井人,朝鲜族,博士,副研究员,主要从事农药环境与毒理研究。E-mail: 1147885795@qq.com

Acute toxicity of cyflumetofen and its metabolites to Daphnia magna Straus

AN Xuehua¹(), LI Dongxue¹, DAI Demao², YU Shifeng², ZHAO Meiqin³, WU Shenggan¹, ZHAO Xueping¹^,^*()

1. Institute of Agro-Product Safety and Nutrition, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021,China
2. Beijing Great-Agri Institute of Pesticide Technology,Beijing 100016, China
3. Beijing Kefa Weiye Technology Limited Company, Beijing 100125, China

Received:2021-05-08 Online:2022-03-25 Published:2022-03-30
Contact: ZHAO Xueping

摘要/Abstract

摘要：

为评价丁氟螨酯及其代谢物[A-2、AB-1 dimer、AB-1、AB-11、B-1、B-3、Target 1(B-2)、Met-1]对水生生物的生态风险,采用半静态法测定丁氟螨酯及其8种代谢物对大型溞48 h暴露的急性毒性效应,以及丁氟螨酯对大型溞的21 d慢性毒性效应。结果表明:丁氟螨酯、Target 1(B-2)和Met-1对大型溞的48 h-EC₅₀(半数抑制浓度)分别为>0.011 5、>0.031 5、>0.032 8 mg·L^-1,在溶解度范围内对大型溞的活动无影响;B-1和B-3对大型溞的48 h-EC₅₀均大于133 mg·L^-1,属于低毒;A-2、AB-1 dimer、AB-1、AB-11的48 h-EC₅₀分别为7.20、0.000 127、1.71、0.316 mg·L^-1,分别属于中毒、剧毒、中毒和高毒。丁氟螨酯对大型溞的21 d无可观察效应浓度(NOEC)大于0.017 8 mg·L^-1,说明其在溶解度范围内对大型溞的生长和繁殖无显著抑制效应。基于48 h-EC₁₀(10%抑制浓度)和48 h-EC₅₀计算急慢性毒性比(ACR),A-2、AB-1 dimer、AB-1、AB-11的ACR值范围为0.235~1.60,远小于推荐值(100)。综上,丁氟螨酯在溶解度范围内对大型溞无明显的急性毒性和慢性毒性,但代谢物中的A-2、AB-1 dimer、AB-1和AB-11会抑制大型溞急性活动,其环境风险不容忽视。研究结果可为丁氟螨酯的水生态风险评价和该类农药的合理安全使用提供基础数据。

关键词: 丁氟螨酯, 大型溞, 急性毒性, 慢性毒性

Abstract:

To evaluate the risk of cyflumetofen and its metabolites on aquatic organisms, acute toxicities of cyflumetofen and its metabolites [A-2, AB-1 dimer, AB-1, AB-11, B-1, B-3, Target 1(B-2), Met-1] on Daphnia magna Straus within 48 h were carried out by semi-static tests, and chronic toxicities of cyflumetofen on D. magna were also investigated by 21 d exposure tests. It was shown that the 48h-EC₅₀ (50% inhibitory concentration) of cyflumetofen, Target 1 (B-2) and Met-1 on D. magna were>0.011 5, >0.031 5,>0.032 8 mg·L^-1, respectively, indicating that these reagents had no effect on the activity of D. magna in the concentration range of solubility. The 48 h-EC₅₀ of B-1 and B-3 were both higher than 133 mg·L^-1, indicating low toxicity. The 48 h-EC₅₀ of A-2, AB-1 dimer, AB-1 and AB-11 were 7.20, 0.000 127, 1.71, 0.316 mg·L^-1, respectively, indicating medium toxicity, very high toxicity, medium toxicity and high toxicity.The no observable effect concentration (NOEC) of D. magna continuously exposed for 21 d was less than 0.017 8 mg·L^-1, indicating that the cyflumetofen had no significant inhibitory effect on the growth and reproduction of D. magna in the maximum solubility.Based on 48 h-EC₁₀ (10% inhibitory concentration) and 48 h-EC₅₀, the acute-chronic toxicity ratio (ACR) was calculated.The determined ACRs of A-2, AB-1 dimer, AB-1 and AB-11 ranged from 0.235 to 1.60, which were much lower than the recommended values (100). In conclusion, cyflumetofen within the maximum solubility had no acute and chronic toxic effects on D. magna, but its metabolites A-2, AB-1 dimer, AB-1 and AB-11 had adverse effects,of which the environmental risk should never be neglected.The present results provided scientific basis for the assessment of aquatic environment risk and safe use of cyflumetofen.

Key words: cyflumetofen, Daphnia magna Straus, acute toxicity, chronic toxicity

中图分类号:

S481.8

安雪花, 李冬雪, 代德茂, 余世锋, 赵美芹, 吴声敢, 赵学平. 丁氟螨酯及其代谢物对大型溞的毒性效应[J]. 浙江农业学报, 2022, 34(3): 557-565.

AN Xuehua, LI Dongxue, DAI Demao, YU Shifeng, ZHAO Meiqin, WU Shenggan, ZHAO Xueping. Acute toxicity of cyflumetofen and its metabolites to Daphnia magna Straus[J]. Acta Agriculturae Zhejiangensis, 2022, 34(3): 557-565.

图/表 9

参考文献 21

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药剂 Reagent	流动相 Mobile phase	流速 Flow rate/ (mL·min^-1)	进样体积 Injection volume/μL	保留时间 Retention time/min
丁氟螨酯	0.1%甲酸水溶液和乙腈	0.25	5.00	4.782
Cyflumetofen	0.1% formic acid aqueous solution and acetonitrile
A-2	2 mmol·L^-1乙酸铵水溶液和甲醇	0.50	20.00	2.092
	2 mmol·L^-1 ammonium acetate aqueous solution and methanol
AB-1 dimer	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	2.00	3.727
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
AB-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.251
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
AB-11	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.482
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
B-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	5.00	2.009
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
B-3	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	2.155
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
Tagrte 1(B-2)	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	2.00	2.944
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
Met-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.403
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol

药剂 Reagent	流动相 Mobile phase	流速 Flow rate/ (mL·min^-1)	进样体积 Injection volume/μL	保留时间 Retention time/min
丁氟螨酯	0.1%甲酸水溶液和乙腈	0.25	5.00	4.782
Cyflumetofen	0.1% formic acid aqueous solution and acetonitrile
A-2	2 mmol·L^-1乙酸铵水溶液和甲醇	0.50	20.00	2.092
	2 mmol·L^-1 ammonium acetate aqueous solution and methanol
AB-1 dimer	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	2.00	3.727
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
AB-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.251
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
AB-11	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.482
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
B-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	5.00	2.009
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
B-3	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	2.155
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol
Tagrte 1(B-2)	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和乙腈	0.30	2.00	2.944
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and acetonitrile
Met-1	0.1%甲酸+2 mmol·L^-1甲酸铵水溶液和甲醇	0.30	2.00	3.403
	0.1% formic acid+2 mmol·L^-1 ammonium formate aqueous solution and methanol

药剂 Reagent	母离子 Parent ion(m/z)	子离子 Daughter ion(m/z)	驻留时间 Dwell time/ms	去簇电压 Declustering potential/V	碰撞能量 Collision energy/V
丁氟螨酯Cyflumetofen	448.1	173.1(249.1)	100	190	32(12)
A-2	174.1	117.0(91.0)	100	30(40)	38(41)
AB-1 dimer	689.3	288.2(268.1)	100	80	19(40)
AB-1	346.2	250.2(270.1)	100	120	32(19)
AB-11	454.0	368.0(281.0)	100	120	24(27)
B-1	189.0	145.0(69.0)	100	-80	-18(-45)
B-3	190.0	130.0(170.0)	100	80	27(14)
Target 1(B-2)	380.1	173.1(190.0)	100	80	32(14)
Met-1	393.2	173.0(263.0)	100	120	42(17)

药剂 Reagent	母离子 Parent ion(m/z)	子离子 Daughter ion(m/z)	驻留时间 Dwell time/ms	去簇电压 Declustering potential/V	碰撞能量 Collision energy/V
丁氟螨酯Cyflumetofen	448.1	173.1(249.1)	100	190	32(12)
A-2	174.1	117.0(91.0)	100	30(40)	38(41)
AB-1 dimer	689.3	288.2(268.1)	100	80	19(40)
AB-1	346.2	250.2(270.1)	100	120	32(19)
AB-11	454.0	368.0(281.0)	100	120	24(27)
B-1	189.0	145.0(69.0)	100	-80	-18(-45)
B-3	190.0	130.0(170.0)	100	80	27(14)
Target 1(B-2)	380.1	173.1(190.0)	100	80	32(14)
Met-1	393.2	173.0(263.0)	100	120	42(17)

药剂 Reagent	回归方程 Regression equation	相关系数 Correlation coefficient	检出限 Limit of quantitation/ (mg·L^-1)	添加浓度 Added concentration/ (mg·L^-1)	回收率 Recovery rate/%	相对标准偏差 Relative standard deviation/%
丁氟螨酯	y=91 649 764x+87 584	0.998 5	0.002 00	0.002 00,0.200	102~105	2.01,1.97
Cyflumetofen
A-2	y=77 557x-537	0.999 8	0.100 00	1.00	94.1~101	2.35
AB-1 dimer	y=8 671 983x+9 807	0.999 4	0.000 10	0.005 00	84.1~104	1.24
AB-1	y=108 411 549x+10 241	0.999 8	0.002 00	2.00	92.2~92.5	5.89
AB-11	y=34 137 757x+28 128	0.999 1	0.002 00	2.00	78.8~83.8	3.87
B-1	y=97 291 050x+4 500	0.999 9	0.002 00	45.6,160	99.7~100	1.34,1.07
B-3	y=346 495 965x+45 040	0.999 9	0.001 00	42.0,168	96.0~102	7.34,1.04
Target 1(B-2)	y=53 024 767x+57 544	0.998 7	0.002 00	52.0	91.0~96.9	1.43
Met-1	y=2 574 847 778x+44 275	0.999 9	0.001 00	2.00	95.2~95.8	3.86

丁氟螨酯及其代谢物对大型溞的毒性效应

Acute toxicity of cyflumetofen and its metabolites to Daphnia magna Straus

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药剂 Reagent	试验浓度 Theoretical concentration	实测浓度1 Measured concentration 1	实测浓度2 Measured concentration	平均浓度 Mean concentration
丁氟螨酯Cyflumetofen	50.0	0.064 6	0.002 06	0.011 5
A-2	25.0	13.3	14.8	14.0
	20.8	10.6	11.7	11.1
	17.4	9.23	8.74	8.98
	14.5	7.82	6.73	7.25
	12.1	6.64	5.44	6.01
	10.0	5.41	5.09	5.25
	8.37	3.72	4.22	3.96
AB-1 dimer	15.1	0.000 185	0.000 255	0.000 217
	12.6	0.000 146	0.000 148	0.000 147
	10.5	0.000 144	0.000 139	0.000 141
	8.71	0.000 112	0.000 107	0.000 109
	7.30	0.000 140	0.000 122	0.000 131
	6.06	ND	ND	—
AB-1	22.0	3.10	2.93	3.01
	18.2	2.39	2.27	2.33
	15.0	1.98	2.17	2.07
	12.4	1.50	1.55	1.52
	10.3	1.26	1.39	1.32
	8.50	1.13	1.09	1.11
	7.01	0.906	0.984	0.944
AB-11	420	0.548	0.298	0.404
	356	0.526	0.274	0.380
	302	0.473	0.266	0.355
	255	0.445	0.206	0.303
	217	0.413	0.206	0.292
B-1	120	136	131	133
B-3	130	143	124	133
Target 1(B-2)	400	0.031 5	ND	—
Met-1	400	0.045 0	0.023 9	0.032 8

t/d	实测浓度 Measured concentration/(mg·L^-1)	t/d	实测浓度 Measured concentration/(mg·L^-1)
0	0.066 5	4^-	0.002 50
1^-	0.002 54	4⁺	0.053 2
1⁺	0.051 0	5^-	0.002 61
2^-	0.002 39	14⁺	0.054 5
2⁺	0.060 5	15^-	0.002 48
3^-	0.002 54	20⁺	0.062 6
3⁺	0.065 2	21	0.002 27

药剂 Reagent	回归方程 Regression equation	相关系数 Correlation coefficient	EC₅₀/ (mg·L^-1)	95%置信区间 95% confidential interval/(mg·L^-1)	毒性类别 Toxicity level
丁氟螨酯Cyflumetofen	—	—	>0.011 5	—	—
A-2	Y=0.359 5+6.249 1X	0.993 2	7.20	6.90~7.51	中毒Medium toxicity
AB-1 dimer	Y=18.499 2+3.464 3X	0.929 6	0.000 127	0.000 106~0.000 151	剧毒Very high toxicity
AB-1	Y=3.761 2+5.302 1X	0.969 1	1.71	1.56~1.87	中毒Medium toxicity
AB-11	Y=10.004 5+10.069 0X	0.959 0	0.316	0.297~0.335	高毒High toxicity
B-1	—	—	>133	—	低毒Low toxicity
B-3	—	—	>133	—	低毒Low toxicity
Tagrte 1(B-2)	—	—	>0.031 5	—	—
Met-1	—	—	>0.032 8	—	—

处理 Treatment	实测浓度 Measured concentration/ (mg·L^-1)	亲溞数量 Number of parent daphnia	亲溞死亡率 Mortality of parent daphnia/%	亲溞初次生殖时间 Time of the first presenting offspring/d	每只亲溞生殖总胎数 Number of brood per parent daphnia	每只亲溞所产存活幼溞总数 Total number of living offspring	每只存活亲溞体长 Body length of living parent daphnia/mm
试验组	0.017 8	12	0	7.00±0.70	8.88±1.21	382±32	3.477±0.186
Experiment group
对照组	—	24	0	6.81±0.71	9.08±0.98	373±25	3.505±0.072
Control group

药剂 Reagent	EC₁₀/ (mg·L^-1)	EC₅₀/ (mg·L^-1)	ACR
A-2	4.49	7.20	1.60
AB-1 dimer	0.000 540	0.000 127	0.235
AB-1	0.98	1.71	1.74
AB-11	0.238	0.316	1.33

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