Residues of glyphosate and aminomethylphosphonic acid (AMPA) in genetically modified glyphosate tolerant soybean, corn and cotton crops

Rodrigues, Nadia Regina; Souza, Ana Paula Ferreira de; Morais, Pedro Patric Pinho; Braga, Daniella Pascon Vianna; Crivellari, Augusto Cesar; Favoretto, Luís Roberto Graça; Berger, Geraldo Ubirajara

doi:10.1590/0103-8478cr20190244

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CROP PROTECTION • Cienc. Rural 51 (01) • 2021 • https://doi.org/10.1590/0103-8478cr20190244 copy

Residues of glyphosate and aminomethylphosphonic acid (AMPA) in genetically modified glyphosate tolerant soybean, corn and cotton crops

Resíduos de glifosato eácido aminometilfosfônico (AMPA) em culturas de soja, milho e algodão geneticamente modificados tolerantes ao glifosato

Authorship SCIMAGO INSTITUTIONS RANKINGS

ABSTRACT:

Glyphosate is a broad-spectrum herbicide capable of controlling a wide range of weed. It uses could cause the occurrence of residues in conventional or genetically modified crops. For this purpose, grains (soybean and corn) and cotton seeds were sampled from commercial areas in 2012/2013 to 2017/2018 seasons in different Brazilian agricultural regions to monitor glyphosate residues levels and its metabolite (aminomethylphosphonic acid - AMPA) after different managements. The glyphosate residues levels in genetically modified corn (GM) ranged from no detected (ND) to 0.15 mg kg^-1, in GM soybean values ranged from ND to 2.81 mg kg^-1 and in GM cotton ranged from ND to 1.78 mg kg^-1. AMPA residues levels indicated a correlation with the glyphosate residues. Glyphosate residues levels in soybean and corn grains and cotton seeds were within the Maximum Residue Limits (MRLs) established by ANVISA and Codex Alimentarius.

Key words:
monitoring; soybean; corn; cotton; commercial areas

Authorship

Nadia Regina Rodrigues ^*E-mail: nadia@cpqba.unicamp.br. *Corresponding author

Divisão de Química Analítica, Centro de Pluridisciplinar de Pesquisas, Químicas, Biológicas e Agrícolas (CPQBA), Universidade Estadual de Campinas (UNICAMP), 13083-970, Campinas, SP, Brasil..Universidade Estadual de Campinas (UNICAMP)BrazilCampinas, SP, BrazilDivisão de Química Analítica, Centro de Pluridisciplinar de Pesquisas, Químicas, Biológicas e Agrícolas (CPQBA), Universidade Estadual de Campinas (UNICAMP), 13083-970, Campinas, SP, Brasil..

https://orcid.org/0000-0002-5524-9781

Ana Paula Ferreira de Souza

Pedro Patric Pinho Morais

Regulatory Sciences - Crop Sciences Division, Bayer (Monsanto Legacy), São Paulo, SP, Brasil .Bayer (Monsanto Legacy)BrasilSão Paulo, SP, BrasilRegulatory Sciences - Crop Sciences Division, Bayer (Monsanto Legacy), São Paulo, SP, Brasil .

Daniella Pascon Vianna Braga

Augusto Cesar Crivellari

Luís Roberto Graça Favoretto

Geraldo Ubirajara Berger

E-mail: nadia@cpqba.unicamp.br. *Corresponding author

DECLARATION OF CONFLICT OF INTERESTS

The authors declare no conflict of interest. The funding sponsors had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, and in the decision to publish the results.

AUTHORS’ CONTRIBUTIONS

GUB, LRGF and ACC conceived and designed experiments. GBU, LRGF, DPVB, ACC and PPPM supervised the experiments, NRR and APFS carried out the lab analyses. PPPM performed statistical analyses of experimental data. PPPM, DPVB, NRR and APFS prepared the draft of the manuscript. All authors critically revised the manuscript and approved of the final version.

SCIMAGO INSTITUTIONS RANKINGS

Figures | Tables

Figures (3)
Tables (9)

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Figure 1
Schematic presentation of data sets of the following GM products: MON 89034 × NK603 corn (VT PRO2^® ), MON 89034 × MON 88017 corn (VT PRO3^® ), MON 531 × MON 1445 cotton (Bollgard RR^® ), MON 15985 × MON 88913 cotton (Bollgard II RR FLEX^® ) and MON 87701 × MON 89788 soybean (Intacta RR2 Pro^® ).

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Figure 2
Averages of glyphosate and AMPA (mg kg ^-1) residues in treatments MON 89034 × NK603, MON 89034 × MON 88017, MON 531 × MON 1445, MON 15985 × MON 88913, MON 87701 × MON 89788, control 1, control 2, control 3, control 4 and control 5.

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Figure 3
Average of glyphosate residues (mg kg^-1) in soybean and corn grains and cotton seeds. (A) By the number of applications of the herbicide in pre-planting (PP) and post-emergence (PE) of the crop and (B) by the period between last application and harvest (days).

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Table 1
Information about the treatments, crops and study sites.

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Table 2
MON 87701 × MON 89788 soybean: study sites, seasons, treatments, application number, time of application and doses.

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Table 3
MON 89034 × NK603 corn: study sites, seasons, treatments, application number, time of application and doses.

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Table 4
MON 89034 × MON 88017 corn: study sites, seasons, treatments, application number, time of application and doses.

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Table 5
MON 531 × MON 1445 cotton: study sites, seasons, treatments, application number, time of application and doses.

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Table 6
MON 15985 × MON 88913 cotton: study sites, seasons, treatments, application number, time of application and doses.

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Table 7
Glyphosate and AMPA residues levels in corn grains from treatments MON 89034 × NK603, control 1, MON 89034 × MON 88017 and control 2.

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Table 8
Glyphosate and AMPA residues in cotton seeds from treatments MON 531 × MON 1445, control 3, MON 15985 × MON 88913 and control 4.

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Table 9
Glyphosate and AMPA residues in soybean grains from treatments MON 87701 × MON 89788 and control 5.

Figure 1 Schematic presentation of data sets of the following GM products: MON 89034 × NK603 corn (VT PRO2^® ), MON 89034 × MON 88017 corn (VT PRO3^® ), MON 531 × MON 1445 cotton (Bollgard RR^® ), MON 15985 × MON 88913 cotton (Bollgard II RR FLEX^® ) and MON 87701 × MON 89788 soybean (Intacta RR2 Pro^® ).

Figure 2 Averages of glyphosate and AMPA (mg kg ^-1) residues in treatments MON 89034 × NK603, MON 89034 × MON 88017, MON 531 × MON 1445, MON 15985 × MON 88913, MON 87701 × MON 89788, control 1, control 2, control 3, control 4 and control 5.

Figure 3 Average of glyphosate residues (mg kg^-1) in soybean and corn grains and cotton seeds. (A) By the number of applications of the herbicide in pre-planting (PP) and post-emergence (PE) of the crop and (B) by the period between last application and harvest (days).

Table 1 Information about the treatments, crops and study sites.

--------------------------------------------Treatments----------------------------------------		Crop	Season	Study sites^a
GM Technology	Control
MON 89034 × NK603	Conventional Hybrids/glyphosate tolerant (Control 1)^b	Corn	2012/2013 to 2016/2017	ROL and MVD
MON 89034 × MON 88017	Hybrids glyphosate tolerant (Control 2)	Corn	2014/2015 to 2017/2018	ROL and MCT
MON 531 × MON 1445	Conventional Cultivars/glyphosate tolerant (Control 3)^b	Cotton	2012/2013 to 2016/2017	LEM, CAV and PVL
MON 15985 × MON 88913	Cultivars glyphosate tolerant (Control 4)	Cotton	2013/2014 to 2016/2017	LEM, CAV and PVL
MON 87701 × MON 89788	Cultivars glyphosate tolerant (Control 5)	Soybean	2013/2014 to 2017/2018	MCT and PVL

^a MCT: Mato Castelhano, RS; SLG: São Luiz Gonzaga, RS; ROL: Rolândia, PR; PGR: Ponta Grossa, PR; LON: Londrina, PR; MVD: Montividiu, GO; SHG: Santa Helena de Goiás, GO; LEM: Luís Eduardo Magalhães, BA; BAR: Barreiras, BA; RON: Rondonópolis, MT; SOR: Sorriso, MT; PVL: Primavera do Leste, MT; CAV: Campo Verde, MT; SGO: São Gabriel do Oeste, MS.
^b control 1: conventional hybrids were used in the 2012/2013 and 2013/2014 seasons, RR hybrids were used as control 1 in the other seasons; control 3: conventional cultivar was used in the 2012/2013 season, RR cultivars were used as control 3 in the other seasons.

Table 2 MON 87701 × MON 89788 soybean: study sites, seasons, treatments, application number, time of application and doses.

Study sites/Seasons^a	Treatments	Applications number^b	Times^c	Doses (g a.e ha^-1)^d
MCT 2013/2014	MON 87701 × MON 89788 soybean	3	PP; PE	1016; 1080 e 360
MCT 2013/2014	Control 5	3	PP; PE	1016; 1080 e 360
PVL 2013/2014	MON 87701 × MON 89788 soybean	3	PP; PE	1650; 1364 e 909
PVL 2013/2014	Control 5	3	PP; PE	1650; 1364 e 909
MCT 2014/2015	MON 87701 × MON 89788 soybean	1	PE	1189
MCT 2014/2015	Control 5	1	PE	1189
PVL 2014/2015	MON 87701 × MON 89788 soybean	2	PP; PE	975; 911
PVL 2014/2015	Control 5	2	PP; PE	975; 911
MCT 2015/2016	MON 87701 × MON 89788 soybean	2	PP; PE	654; 654
MCT 2015/2016	Control 5	2	PP; PE	654; 654
PVL 2015/2016	MON 87701 × MON 89788 soybean	4	PP; PE	1060; 1300, 845 e 845
PVL 2015/2016	Control 5	4	PP; PE	1060; 1300, 845 e 845
MCT 2016/2017	MON 87701 × MON 89788 soybean	2	PP; PE	1000; 1080
MCT 2016/2017	Control 5	2	PP; PE	1000; 1080
PVL 2016/2017	MON 87701 × MON 89788 soybean	3	PP; PE	1170; 650 e 650
PVL 2016/2017	Control 5	3	PP; PE	1170; 650 e 650
MCT 2017/2018	MON 87701 × MON 89788 soybean	2	PP; PE	576; 1030
MCT 2017/2018	Control 5	2	PP; PE	576; 1030

^a MCT: Mato Castelhano, RS; PVL: Primavera do Leste, MT.
^b,c,d PP: pre-planting; PE: post-emergence; the management used with glyphosate was decided by each farmer responsible for the area in which MON 87701 × MON 89788 soybean study was installed. (g a.e ha^-1): grams of equivalent acid per hectare

Table 3 MON 89034 × NK603 corn: study sites, seasons, treatments, application number, time of application and doses.

Study sites/Seasons^a	Treatments	Applications number^b	Times^c	Doses (g a.e ha^-1)^d
ROL 2012/2013	MON 89034 × NK603 corn	2	PP; PE	722; 981
ROL 2012/2013	Control 1^*	1	PP	722
MVD 2012/2013	MON 89034 × NK603 corn	2	PP; PE	711; 872
MVD 2012/2013	Control 1	1	PP	711
ROL 2013/2014	MON 89034 × NK603 corn	2	PP; PE	1081; 893
ROL 2013/2014	Control 1	1	PP	1081
MVD 2013/2014	MON 89034 × NK603 corn	1	PE	667
MVD 2013/2014	Control 1	-	-	-
ROL 2014/2015	MON 89034 × NK603 corn	2	PP; PE	1440; 1440
ROL 2014/2015	Control 1	1	PP	1440
MVD 2014/2015	MON 89034 × NK603 corn	1	PE	1636
MVD 2014/2015	Control 1	1	PE	1636
ROL 2015/2016	MON 89034 × NK603 corn	2	PP; PE	785; 1011
ROL 2015/2016	Control 1	1	PP	785
MVD 2015/2016	MON 89034 × NK603 corn	2	PP; PE	1200; 1470
MVD 2015/2016	Control 1	1	PP	1200
ROL 2016/2017	MON 89034 × NK603 corn	1	PE	2774
ROL 2016/2017	Control 1	1	PE	2774
MVD 2016/2017	MON 89034 × NK603 corn	1	PE	960
MVD 2016/2017	Control 1	1	PE	960

^a ROL: Rolândia, PR; MVD: Montividiu, GO.
^b,c,d PP: pre-planting; PE: post-emergence; the management used with glyphosate was decided by each farmer responsible for the area in which MON 89034 × NK603 corn study was installed. (g a.e ha^-1): gramsofequivalent acid per hectare.
^*control 1: conventional hybrids were used in the 2012/2013 and 2013/2014 seasons, RR hybrids were used as control 1 in the other seasons.

Table 4 MON 89034 × MON 88017 corn: study sites, seasons, treatments, application number, time of application and doses.

Study sites/Seasons^a	Treatments	Applications number^b	Times^c	Doses(g a.e ha^-1)^d
MCT 2014/2015	MON 89034 × MON 88017 corn	2	PP; PE	1025; 793
MCT 2014/2015	Control 2	2	PP; PE	1025; 793
ROL 2014/2015	MON 89034 × MON 88017 corn	2	PP; PE	1440; 1440
ROL 2014/2015	Control 2	1	PP	1440
MCT 2015/2016	MON 89034 × MON 88017 corn	2	PP; PE	720; 654
MCT 2015/2016	Control 2	2	PP; PE	720; 654
ROL 2015/2016	MON 89034 × MON 88017 corn	2	PP; PE	785; 654
ROL 2015/2016	Control 2	2	PP; PE	785; 654
ROL 2016/2017	MON 89034 × MON 88017 corn	1	PE	2774
ROL 2016/2017	Control 2	1	PE	2774
MCT 2017/2018	MON 89034 × MON 88017 corn	2	PP; PE	781; 936
MCT 2017/2018	Control 2	2	PP; PE	781; 936
ROL 2017/2018	MON 89034 × MON 88017 corn	2	PP; PE	518; 2160
ROL 2017/2018	Control 2	2	PP; PE	518; 2160

^a MCT: Mato Castelhano, RS; ROL: Rolândia, PR.
^b,c,d PP: PP: pre-planting; PE: post-emergence; the management used with glyphosate was decided by each farmer responsible for the area in which MON 89034 × MON 88017 corn study was installed. (g a.e ha^-1): grams of equivalent acid per hectare.

Table 5 MON 531 × MON 1445 cotton: study sites, seasons, treatments, application number, time of application and doses.

Study sites/Seasons^a	Treatments	Applicatios number^b	Times^c	Doses (g a.e ha^-1)^d
LEM 2012/2013	MON 531 × MON 1445 cotton	1^**	PE	1817
LEM 2012/2013	Control 3^*	-	-	-
PVL 2013/2014	MON 531 × MON 1445 cotton	3	PP; PE	1440; 1111 e 1111
PVL 2013/2014	Control 3	3	PP; PE	1440; 1111 e 1111
PVL 2014/2015	MON 531 × MON 1445 cotton	3	PP; PE	1430; 975 e 1441
PVL 2014/2015	Control 3	2	PP; PE	1430; 975
LEM 2015/2016	MON 531 × MON 1445 cotton	2	PP; PE	1500; 1250
LEM 2015/2016	Control 3	2	PP; PE	1500; 1250
CAV 2015/2016	MON 531 × MON 1445 cotton	2	PP; PE	900; 900
CAV 2015/2016	Control 3	2	PP; PE	900; 900
LEM 2016/2017	MON 531 × MON 1445 cotton	3	PP; PE	1500; 1000 e 1000
LEM 2016/2017	Control 3	3	PP; PE	1500; 1000 e 1000
CAV 2016/2017	MON 531 × MON 1445 cotton	2	PP; PE	1296; 1440
CAV 2016/2017	Control 3	2	PP; PE	1296; 1440

^a LEM: Luís Eduardo Magalhães, BA; PVL: Primavera do Leste, MT; CAV: Campo Verde, MT.
^b,c,d PP: pre-planting; PE: post-emergence; the management used with glyphosate was decided by each farmer responsible for the area in which MON 531 × MON 1445 cotton study was installed. (g a.e ha^-1): gramsofequivalent acid per hectare.
^*control 3: conventional cultivar was used in the 2012/2013 season; RR cultivars were used as control 3 in the other seasons. ^**Partial information obtained from the farmer.

Table 6 MON 15985 × MON 88913 cotton: study sites, seasons, treatments, application number, time of application and doses.

Study sites/Seasons^a	Treatments	Applications number^b	Times^c	Doses (g a.e ha^-1)^d
LEM 2013/2014	MON 15985 × MON 88913 cotton	1	PP	797
LEM 2013/2014	Control 4	2	PP; PE	797; 960
LEM 2015/2016	MON 15985 × MON 88913 cotton	2	PP; PE	1500; 1250
LEM 2015/2016	Control 4	2	PP; PE	1500; 1250
CAV 2015/2016	MON 15985 × MON 88913 cotton	2	PP; PE	900; 900
CAV 2015/2016	Control 4	2	PP; PE	900; 900
CAV 2016/2017	MON 15985 × MON 88913 cotton	2	PP; PE	1296; 1440
CAV 2016/2017	Control 4	2	PP; PE	1296; 1440

^a LEM: Luís Eduardo Magalhães, BA; PVL: Primavera do Leste, MT; CAV: Campo Verde, MT.
^b,c,d PP: pre-planting; PE: post-emergence; the management used with glyphosate was decided by each farmer responsible for the area in which MON 15985 × MON 88913 cotton study was installed. (g a.e ha^-1): grams of equivalent acid per hectare.

Table 7 Glyphosate and AMPA residues levels in corn grains from treatments MON 89034 × NK603, control 1, MON 89034 × MON 88017 and control 2.

Treatments	Study sites/Seasons^a	-----------------------Residues (mg kg^-1)-------------------
		Glyphosate	AMPA
MON 89034 × NK603	ROL 2012/2013	ND	ND
Control 1^*	ROL 2012/2013	ND	0.16
MON 89034 × NK603	MVD 2012/2013	ND	ND
Control 1	MVD 2012/2013	ND	<LOQ
MON 89034 × NK603	ROL 2013/2014	0.11	0.49
Control 1	ROL 2013/2014	ND	0.05
MON 89034 × NK603	MVD 2013/2014	0.11	ND
Control 1	MVD 2013/2014	ND	ND
MON 89034 × NK603	ROL 2014/2015	<LOQ	<LOQ
Control 1	ROL 2014/2015	<LOQ	<LOQ
MON 89034 × NK603	MVD 2014/2015	ND	ND
Control 1	MVD 2014/2015	ND	ND
MON 89034 × NK603	ROL 2015/2016	<LOQ	ND
Control 1	ROL 2015/2016	<LOQ	ND
MON 89034 × NK603	MVD 2015/2016	0.06	<LOQ
Control 1	MVD 2015/2016	ND	ND
MON 89034 × NK603	ROL 2016/2017	ND	ND
Control 1	ROL 2016/2017	<LOQ	0.05
MON 89034 × NK603	MVD 2016/2017	0.07	<LOQ
Control 1	MVD 2016/2017	ND	ND
MON 89034 × MON 88017	MCT 2014/2015	0.09	<LOQ
Control 2	MCT 2014/2015	0.11	<LOQ
MON 89034 × MON 88017	ROL 2014/2015	<LOQ	ND
Control 2	ROL 2014/2015	<LOQ	ND
MON 89034 × MON 88017	MCT 2015/2016	ND	ND
Control 2	MCT 2015/2016	ND	ND
MON 89034 × MON 88017	ROL 2015/2016	<LOQ	<LOQ
Control	ROL 2015/2016	0.05	<LOQ
MON 89034 × MON 88017	ROL 2016/2017	<LOQ	ND
Control 2	ROL 2016/2017	<LOQ	ND
MON 89034 × MON 88017	MCT 2017/2018	0.06	0.01
Control 2	MCT 2017/2018	0.09	0.02
MON 89034 × MON 88017	ROL 2017/2018	0.15	<LOQ
Control 2	ROL 2017/2018	0.14	<LOQ

^a MCT: Mato Castelhano, RS; ROL: Rolândia, PR; MVD: Montividiu, GO.
LOQ: Limit of Quantification (0.05 mg kg^-1); ND: Not Detected.
^*control 1: conventional hybrids were used in the 2012/2013 and 2013/2014 seasons; RR hybrids were used as control 1 in the other seasons.

Table 8 Glyphosate and AMPA residues in cotton seeds from treatments MON 531 × MON 1445, control 3, MON 15985 × MON 88913 and control 4.

Treatments	Study sites/Seasons^a	---------------------Residues (mg kg^-1)-------------------
		Glyphosate	AMPA
MON 531 × MON 1445	LEM 2012/2013	1.78	0.06
Control 3^*	LEM 2012/2013	<LOQ	ND
MON 531 × MON 1445	PVL 2013/2014	0.08	ND
Control 3	PVL 2013/2014	ND	ND
MON 531 × MON 1445	PVL 2014/2015	<LOQ	<LOQ
Control 3	PVL 2014/2015	<LOQ	<LOQ
MON 531 × MON 1445	LEM 2015/2016	<LOQ	<LOQ
Control 3	LEM 2015/2016	0.1	ND
MON 531 × MON 1445	CAV 2015/2016	0.46	<LOQ
Control 3	CAV 2015/2016	0.05	<LOQ
MON 531 × MON 1445	LEM 2016/2017	<LOQ	ND
Control 3	LEM 2016/2017	0.62	ND
MON 531 × MON 1445	CAV 2016/2017	0.11	ND
Control 3	CAV 2016/2017	0.07	ND
MON 15985 × MON 88913	LEM 2013/2014	ND	ND
Control 4	LEM 2013/2014	ND	ND
MON 15985 × MON 88913	LEM 2015/2016	0.07	<LOQ
Control 4	LEM 2015/2016	0.1	ND
MON 15985 × MON 88913	CAV 2015/2016	0.13	<LOQ
Control 4	CAV 2015/2016	0.05	<LOQ
MON 15985 × MON 88913	CAV 2016/2017	<LOQ	ND
Control 4	CAV 2016/2017	0.07	ND

^aLEM: Luís Eduardo Magalhães, BA; CAV: Campo Verde, MT; PVL: Primavera do Leste, MT.
LOQ: Limit of Quantification (0,05 mg kg^-1); ND: Not Detected.
^*control 3: conventional cultivar was used in the 2012/2013 season; RR cultivars were used as control 3 in the other seasons

Table 9 Glyphosate and AMPA residues in soybean grains from treatments MON 87701 × MON 89788 and control 5.

Treatments	Study sites/Seasons^a	----------------------Residues (mg kg^-1)-------------------
		Glyphosate	AMPA
MON 87701 × MON 89788	MCT 2013/2014	0.25	0.5
Control 5	MCT 2013/2014	0.23	0.53
MON 87701 × MON 89788	PVL 2013/2014	0.72	1.02
Control 5	PVL 2013/2014	0.36	0.61
MON 87701 × MON 89788	MCT 2014/2015	0.33	0.45
Control 5	MCT 2014/2015	0.35	0.5
MON 87701 × MON 89788	PVL 2014/2015	0.75	0.76
Control 5	PVL 2014/2015	1.02	0.59
MON 87701 × MON 89788	MCT 2015/2016	0.17	0.59
Control 5	MCT 2015/2016	0.20	0.44
MON 87701 × MON 89788	PVL 2015/2016	2.81	3.38
Control 5	PVL 2015/2016	1.42	2.21
MON 87701 × MON 89788	MCT 2016/2017	0.42	0.29
Control 5	MCT 2016/2017	0.46	0.55
MON 87701 × MON 89788	PVL 2016/2017	1.88	2.69
Control 5	PVL 2016/2017	2.26	1.69
MON 87701 × MON 89788	MCT 2017/2018	0.50	0.80
Control 5	MCT 2017/2018	0.82	1.12

a MCT: Mato Castelhano, RS; PVL: Primavera do Leste, MT.

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Residues of glyphosate and aminomethylphosphonic acid (AMPA) in genetically modified glyphosate tolerant soybean, corn and cotton crops

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[1] E-mail: nadia@cpqba.unicamp.br. *Corresponding author