Acta Universitaria

ISSN: 0188-6266
[email protected]
Universidad de Guanajuato
México

Leyva Morales, José Belisario; Valdez Torres, José Benigno; Bastidas Bastidas, Pedro de
Jesús; Angulo Escalante, Miguel Ángel; Sarmiento Sánchez, Juan Ignacio; Barraza Lobo,
Alma Lorena; Olmeda Rubio, Claudia; Chaidez Quiroz, Cristóbal
Monitoring of pesticides residues in northwestern Mexico rivers
Acta Universitaria, vol. 27, núm. 1, enero-febrero, 2017, pp. 45-54
Universidad de Guanajuato
Guanajuato, México

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 ISSN 0188-6266
doi: 10.15174/au.2017.1203

Monitoring of pesticides residues in northwestern

Mexico rivers
Monitoreo de residuos de plaguicidas en ríos del noroeste de México
José Belisario Leyva Morales*, José Benigno Valdez Torres**, Pedro de Jesús Bastidas Bastidas**,
Miguel Ángel Angulo Escalante**, Juan Ignacio Sarmiento Sánchez***, Alma Lorena Barraza Lobo**,
Claudia Olmeda Rubio**, Cristóbal Chaidez Quiroz**◊
ABSTRACT
In Mexico, use of river water for households, agriculture and industry has adversely af-
fected aquatic environment through chemical and microbial contamination. The aim of this
study was to determine pesticide residues levels in water of rivers from central Sinaloa State,
Northwestern Mexico. In samples obtained from July 2008 to June 2009 pesticides residues
detected were lindane, heptachlor, endosulfan, dicloro difenil tricloroetano (DDT), diazinon,
chlorpyrifos, permethrin, methyl parathion, cyromazine, ethion, carbofenothion, lambda cy-
halotrine, pyrimicarb, malathion and aldrin. None exceeded water quality ecological criteria
or those established by US Environmental Protection Agency. Comparatively low concentra-
tions and frequencies suggest that pesticide contamination derived from runoffs toward
river from contaminated soil particles and not from use of pesticides in intensive agriculture
of region.

RESUMEN
En México, el uso de agua de río para los hogares, la agricultura y la industria ha afectado
negativamente al medio ambiente acuático a través de la contaminación química y micro-
biana. El objetivo de este estudio fue determinar los niveles de residuos de plaguicidas en
agua de ríos del centro de Sinaloa, noroeste de México. En las muestras obtenidas de julio
2008 a junio de 2009, los residuos de plaguicidas detectados fueron lindano, heptacloro,
endosulfán, dicloro difenil tricloroetano (DDT), diazinón, clorpirifos, permetrina, paratión
metílico, ciromazina, etión, carbofenotión, lambda cialotrina, pirimicarb, malatión y aldrin.
Ninguno superó los criterios ecológicos para la calidad del agua o de los establecidos por
la Agencia de Protección Ambiental de Estados Unidos de América. Las concentraciones y
frecuencias relativamente bajas sugieren que la contaminación por plaguicidas derivada de
escurrimientos hacia el río de las partículas de suelo contaminado y no del uso de plagui-
cidas en la agricultura intensiva de la región.
Recibido: 3 de febrero 2016
Aceptado: 16 de noviembre 2016
INTRODUCTION

Keywords:
World’s human population has increased nearly fourfold in the past 100 years.
Agriculture; water; chemical contamination; It is projected to exceed 9 billion by 2050 (Food and Agriculture Organiza-
Culiacan Valley. tion [FAO], 2011). Nearly 40% of the world’s potential crop production is
Palabras clave: lost each year because of weeds, pests and diseases effects (FAO, 2011), an
Agricultura; agua; contaminación argument for use of pesticides for crop protection.
química; Valle de Culiacán.
Besides agricultural applications, pesticides are used to mitigate pres-
ence of organisms that are potentially harmful to human health, especially in
Cómo citar:
Leyva Morales, J. B., Valdez Torres, J. B., countries with tropical climates (World Health Organization [WHO], 2010).
Bastidas Bastidas, P. J., Angulo Escalante, M. Pesticides are systematically used in agriculture, industry, households, gar-
A., Sarmiento Sánchez, J. I., Barraza Lobo, A. L., dens, and veterinary medicine (Comisión Intersecretarial para el control de pro-
Olmeda Rubio, C., & Chaidez Quiroz, C. (2017).
Monitoring of pesticides residues in northwestern
ceso y uso de plaguicidas, fertilizantes y sustancias tóxicas [Cicoplafest], 2004).
Mexico rivers. Acta Universitaria, 27(1), 45-54. Benefits of pesticide use are many; however, dispersion of large amounts to
doi: 10.15174/au.2017.1203 environment adversely affects ecosystems as well as human health (Aktar,
Sengupta & Chowdhury, 2009).
* Consejo Nacional de Ciencia y Tecnología-Universidad Autónoma de Nayarit, Secretaría de Investigación y Posgrado, Centro Nayarita de Innovación y Transferencia de Tecnología, A.C.
(CENITT). Av. Emilio M. González s/n, Col. Cd. Industrial, Tepic, Nayarit, México, C.P. 63173. Tel.: +52(311) 4 56 67 41. Correo electrónico: [email protected]
** Centro de Investigación en Alimentación y Desarrollo, A.C. Carretera a Eldorado km. 5.5, Campo el Diez, Culiacán, Sinaloa, México, C.P. 80129.
*** Facultad de Ingeniería, Universidad Autónoma de Sinaloa. Blvd. de las Américas s/n, Ciudad Universitaria, Culiacán, Sinaloa, México, C.P. 80040.
◊
Corresponding author.

Vol. 27 No. 1 Enero-Febrero 2017 45

 ISSN 0188-6266

Culiacan city, capital of the state of Sinaloa in reaching agricultural fields, subjecting it to various
northwestern Mexico, lies on a plain that includes opportunities for pesticide contamination (Junta Mu-
more than 130 000 ha of crops (42 000 km2 of inten- nicipal de Agua Potable y Alcantarillado de Culiacan
sive agriculture) representing 42% of Sinaloa State and [JAPAC], 2001).
4% of farmland in Mexico. Large quantities of fertiliz-
ers and pesticides are applied there (Ruiz-Fernández, It is important to monitor pesticides in nearby eco-
Páez-Osuna, Hillaire-Marcel, Soto-Jiménez & Ghaleb, systems to agricultural areas to know the impact of
2001). Sinaloa State is a semiarid region, with rainfall agriculture on the environment. The objective of this
events from June to September (mean annual precipi- study was to monitor presence and levels of pesti-
tation 640 mm) and dryness rest of year (Instituto Na- cides in Culiacan, Humaya and Tamazula rivers from
cional de Estadística y Geografía [INEGI], 2011). July 2008 to June 2009. This is one of the first moni-
toring of pesticides in Culiacan Valley’s water, an
Culiacan River Basin is in Hydrological Region extremely important national agricultural region.
010, in northwestern of Mexico, with a surface area
of 18 800 km2, and is formed by Tamazula and Hu-
maya rivers confluence in Culiacan city. Culiacan River MATERIALS AND METHODS
crosses Navolato city and empties into Altata-Ensenada
del Pabellon Lagoon (AEPL) in El Castillo village, Navolato
(Comisión Nacional del Agua [Conagua], 2004), where Sampling sites
intensive farming of shrimp (Penaeus spp.), oysters
(Crassostrea spp.), mussels (Chione spp.) and fish (e.g. Six sampling sites (figure 1) were selected on basis of
Mugil spp., Gerres spp., Lutjanus spp.) produces about existence of farming activities and/or natural run-
3000 t per year. This lagoon system has been extensive- off (streams, canals, etc.). Sites A and B lay on upper
ly studied and high levels of phosphorus, heavy met- reaches of Humaya River (Agua Caliente town, 24°52’07’’
als and pesticides have been documented (Carvalho, N 107°23’28’’ W) and Tamazula River (Jotagua town,
Fowler, González-Farías, Mee & Readman, 1996; Car- 24°51’52’’ N 107°16’12’’ W) respectively, where effects
valho et al., 2002; Galindo-Reyes, Villagrana-Lizárraga, of agricultural activity were minimal. Sites C, D, E and
Guerrero-Ibarra & Quezada-Urenda, 1992; Galindo- F represented agricultural land that forms Culiacan
Reyes, Fossato, Villagrana-Lizarraga & Dolci, 1999a; Valley (20°40’N 107°30’W) from confluence of Humaya
Galindo-Reyes, Villagrana-Lizárraga & Lazcano-Álvarez, and Tamazula rivers: C, sub basin of Culiacan River
1999b; Green-Ruiz & Páez-Osuna, 2001; Páez-Osuna, [Puente Negro (24°48’33’’ N 107°24’28’’ W); D, Co-
Osuna-López, Izaguirre-Fierro & Zazueta-Padilla, fradía de Navolato (24°48’01’’ N 107°36’60’’ W); E, Ira-
1993a; b; Páez-Osuna, Osuna-López, Izaguirre-Fierro & guato (24°37’27’’ N 107°39’52’’ W); and F, El Castillo
Zazueta-Padilla, 1994; Páez-Osuna, Bojórquez-Leyva (24°29’60’’ N 107°42’28’’ W).
& Green-Ruiz, 1998; Ruiz-Fernández et al., 2001;
Ruiz-Fernández, Hillaire-Marcel, Ghaleb, Soto-Jiménez
& Páez-Osuna, 2002; Ruiz-Fernández, Hillaire-
Marcel, Páez-Osuna, Ghaleb & Soto-Jiménez, 2003),
including clear evidence of eutrophication problems
(De la Lanza & Flores-Verdugo, 1998).

Region exports vegetable crops to USA each year,

particularly tomatoes and bell peppers. The lower ba-
sin of Culiacan River combines the highest economic
returns of the two most important economic activities
of the State of Sinaloa, crop production and livestock:
approximately 47 848 ha are under crop production
(tomato, cucumber, bell pepper, and eggplant) and
there are more than 30 cattle farms (INEGI, 2011). Irri-
gation system on these farms is provided by a series of
canals derived from Humaya and Tamazula rivers con-
junction into Culiacan River, which crosses Culiacan Figure 1. Sampling sites in rivers of Culiacan River basin, Sinaloa, Mexico.
city (population, approximately one million) before Source: Author’s own elaboration.

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
46 Vol. 27 No. 1 Enero-Febrero 2017 Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
 ISSN 0188-6266

Sample collection with samples and pH was adjusted to 7.0 by addition

of HCl or NaOH (solution 0.1 M) when was necessary
Fresh surface water was collected, to a 30 cm depth, (Environmental Protection Agency [EPA], 1995a; b).
twice a month from each sampling site over a period of
one year (June 2008 to July 2009) (Mejias & Jerez, 2006). Extraction of pesticides
Samples, in 1 L amber glass containers, were placed in
an ice chest that excluded light, and were transported
Each 1 L water sample was combined with 150 g of so-
to the National Food Safety Research Laboratory at the
dium chloride and stirred in a separatory funnel until
Center of Research for Food and Development (CIAD,
dissolved. Mixture was extracted with dichlorometh-
for its acronym in spanish Culiacan Unit) and stored at
ane (3 mL × 60 mL), shaken for 2 min and allowed
4 ºC until pesticide extraction. In order to avoid biologi-
to stand for 10 minutes to achieve phase separation.
cal degradation of pesticides, extraction was performed
Extracts were combined, dried with anhydrous sodi-
within 48 h of sample collection.
um sulfate and collected in a 500 mL Kuderna-Danish
concentrator, then attached to a 10 mL collection tube
Analysis of pesticides (EPA, 1995a; b) and concentrated in a steam bath. Later,
azeotropic distillation used petroleum ether (150 mL)
Samples were analyzed in two gas chromatographs and acetone (30 mL). Finally, extract was concentrated
Varian 3800 and CP3800 (GC), equipped with; electron until 1 mL of acetone (McMahon & Hardin, 1998).
capture detector (ECD), thermionic specific detector
(TSD), electrolytic conductivity detector (ELCD) and
Method Validation
pulsed flame photometric detector (PFPD). In all cases,
certified reference materials (analytical standards of
pesticides) were used (Chem Service, USA). Solvents Quality control of analytical method was based on re-
(acetone, dichloromethane, hexane and petroleum covery rates of fortified matrix samples (distilled water)
ether) were pesticide grade (Burdick & Jackson®) pur- with groups representing pesticide organochlorines, or-
chased from a local supplier (Sumilab, Mexico). Chro- ganophosphates, synthetic pyrethroids and methylcar-
matographic conditions of analysis for each pesticides bamates. Fortification levels ranged from 0.065 µg/L to
group are shown in table 1. Pesticides were detected 5.58 µg/L. Recovery rates ranged from 70% to 114%
in an initial chromatographic run and confirmed with and relative standard deviation (RSD) was <13% for all
another detector. Methods 507 and 508 reported by US added analytes. Limits of detection (LOD) and quan-
Environment Protection Agency (US EPA) were used for tification (LOQ) were calculated by radio signal/noise
pesticide quantification. ratio (S/N or Np-p) method proposed by the Interna-
tional Conference on Harmonization (ICH, 1996). LOD
Sample preparation were between 0.001 µg/L and 0.059 µg/L, and quanti-
fication limits were three times LOD (table 2). Results
Water samples were filtered through a Whatman #2 fil- were within range suggested by EURACHEM Guide
ter paper. Filtrate and 50 mL PBS 2M were combined (Magnusson & Örnemark, 2014).

Table 1.
Chromatographic conditions for pesticides groups.
Chromatographic Conditions Organophosphates Organochlorines and Pyrethroids Organonitrogens

Detector PFPD ECD TSD

Column CP SIL 5CB de 30 m × 0.53 mm CP SIL 5CB de 25 m × 0.32 mm HP 5 de 25 m × 0.53 mm

Temperature of detector 250 ºC 300 ºC 300 ºC

Temperature of injector 240 ºC 230 ºC 250 ºC

Gas carrier Nitrogen Nitrogen Nitrogen

Volume injected 2 µL 1 µL 2 µL

Source: Author’s own elaboration.

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
Vol. 27 No. 1 Enero-Febrero 2017 47
 ISSN 0188-6266

Table 2. RESULTS
Parameters used for the evaluation of the analytical method.
Pesticide Recovery (%) RSD (%) LOD LOQ
Frequencies and concentration levels
Dimethoate 80.3 5 0.015 0.045
of pesticides in water samples
Diazinon 70 12.9 0.015 0.045

Malathion 81.1 8.2 0.015 0.045

Of 144 water samples analyzed, 24 were taken from
Tamazula River, 24 from Humaya River and 96
Propachlor 71.5 5.8 0.001 0.003 from Culiacan River. Pesticides were present in 81%
Atrazine 78.45 12.9 0.01 0.059 (116/144) of analyzed samples. Their frequencies are
shown in figure 2. Around the world, pesticides moni-
Metalaxyl 78.5 9.6 0.01 0.059
toring in natural environments are important by al-
Lindane 106.65 5.8 0.001 0.003 lows early detection of problems with products toxicity
Heptachlor 89.325 9.6 0.001 0.003
used to control pests and alterations or disturbances
generated in environment. Previous studies show that
Aldrin 70.1 1.9 0.001 0.003 pesticides presence in water is very variable, however
Dichloropropanilide 95.775 12.9 0.001 0.003 most published studies show that >50% of samples
contain at least one pesticide. For example, Picó et al.
pp DDE 108.575 9.6 0.001 0.003
(1994) found pesticides (organochlorines, carbamates,
Endosulfan beta 113.825 12.6 0.001 0.003 triazines and organophosphates) in 62.5% (25/40) of
Cis permethrin 78.225 9.6 0.001 0.003
water samples from rivers Canyoles, Albaida, Claria,
Serpis, Polop, Belcaire, Turia and Xuquer, Lake Al-
Trans permethrin 81.275 9.6 0.001 0.003 bufera and irrigation canals on south coast of Spain,
Carbaryl 79.125 5 0.059 0.177 in the most important agricultural area in Valencia.
Besides, Darko, Akoto & Oppong (2008) reported pres-
Source: Author’s own elaboration. ence of organochlorines pesticides in water samples
from Bosomtwi Lake, Ghana. DDT was detected in
66% (33/50), lindane in 64% (32/50) and endosulfan
in 56% (28/50) at mean concentrations of 0.012 ng/g,
0.071 ng/g and 0.064 ng/g, respectively.

Presence of pesticides in water samples is highly

variable and may depend on many factors including
sample size, number of samples analyzed; extraction
method used and most important use of pesticides
in study area. Similarly, most studies show a positive
sample percentage above 50% for at least one pesti-
cide (Darko, Akoto & Oppong, 2008; Picó et al., 1994).

In the present study, 15% of positive samples

(21/144) were from Tamazula River, 12% (17/144)
from Humaya River and 73% (106/144) from Culia-
can River. The highest percentage of samples contain-
ing pesticide residues corresponded to Culiacan River.
This may be related to the large area of intensive agri-
culture in Culiacan River lower basin.

Concentrations of pesticides (table 3) were within

range permitted by ecological standards of water quality
Figure 2. Frequency of individual pesticides detected in 144 water samples from
in Mexico (Diario Oficial de la Federación [DOF], 1989),
six sites in Culiacan River basin. and were below levels permitted by US EPA regarding
Source: Author’s own elaboration. protection of freshwater aquatic life (EPA, 2006).

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
48 Vol. 27 No. 1 Enero-Febrero 2017 Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
 ISSN 0188-6266

Table 3.
Concentrations of pesticides in river water samples from the Culiacan river basin.
Tamazula River Humaya River Culiacan River CE-CCAb EPAc
Pesticide
(µg/L)a ± S.D. (µg/L)a ± S.D. (µg/L)a ± S.D. (µg/L) (µg/L)
Diazinon 0.0296 ± 0.01 [6] 0.0211 ± 0.01 [4] 0.0403 ± 0.02 [28] _ 0.17
Chlorpyrifos 0.0296 ± 0.01[2] 0.0163 ± 0.007 [8] 0.0157 ± 0.01 [32] _ 0.083
DDT 0.05102 ± 0.04[7] 0.0525 ± 0.05 [10] 0.0425 ± 0.05 [32] 1 1.1
Endosulfan 0.03601 ± 0.03[18] 0.0201 ± 0.01 [12] 0.0198 ± 0.01 [44] 0.2 0.22
Ethion N.D. N.D. 0.0162 ± 0.006 [4] _ _
Aldrin 0.0229 ± 0.01[6] 0.0099 ± 0.00 [1] 0.1023 ± 0.16 [7] 3 3
Heptachlor 0.0377 ± 0.02[4] N.D. 0.0059 ± 0.01 [4] 0.5 0.52
Lindane 0.0104 ± 0.001[5] 0.0041 ± 0.00 [1] 0.0045 ± 0.003 [7] 2 0.95
Carbaryl N.D. N.D. 0.1113 ± 0.00 [1] _ _
Carbophenothion N.D. N.D. 0.0099 ± 0.00 [1] _ _
Permethrin N.D. N.D. 0.2351 ± 0.18[7] _ _
Methyl Parathion 0.0036 ± 0.00[1] N.D. 0.0098 ± 0.004 [6] 0.04 0.065
Cyromazine 0.1177 ± 0.00[1] N.D. 0.1961 ± 0.00 [1] _ _
Pirimicarb N.D. N.D. 0.0772 ± 0.00 [1] _ _
Malathion 0.0059 ± 0.0302[5] N.D. N.D. _ 0.1
Lamda Cyhalothrin N.D. 0.0212 ± 0.00 [1] N.D. _ _

a
: Mean concentration; [ ]: indicates number of concentrations; S.D.: Standard Deviation; b: CCE-CCA, Ecological Criteria for Water Quality, DOF (1989); c: EPA, Envi-
ronmental Protection Agency; N.D.: Not Detected.
Source: Author’s own elaboration.

The highest concentration of pesticides in Tamazula of detritus and then undergoes microbial degradation
River occurred during July and corresponded to DDT to become DDE (dichlorodiphenyldichloroethylene)
(0.156 µg/L) and endosulfan (0.156 µg/L). For Humaya (Aislabie, Richards & Boul, 1997; Miglioranza, Aizpún
River, the highest concentration also occurred in July & Moreno, 2003).
and corresponded to DDT (0.167 µg/L). In Culiacan
River, the maximum concentration of pesticides dif- Organochlorines (OCs)
fered among sampling sites. At site C the highest con-
Frequencies of detection of organochlorine pesticides in
centrations were cyromazine (0.196 µg/L) in September samples were, in descending order, endosulfan (41%)>
and DDT (0.286 µg/L) in July; at site D the highest was DDT (27.1%)> aldrin (8.3%)> lindano (6.3%)> hepta-
aldrin (0.462 µg/L) in January; at site E the highest chlor (2.8%) (figure 2).
was carbaryl (0.111 µg/L) in July; and at site F the
highest was diazinon (0.124 µg/L) in September. Persistence and movement of pesticides in envi-
ronment are determined by characteristics such as
Concentration of pesticide residues did not differ water solubility, octanol-water partition coefficient
significantly among sampling sites, mainly because (Kow), organic carbon sorption constant (Koc), Henry’s
constant movement and exchange of water masses law constant and half-life (DT50) (table 4).
through system caused mixing and homogenization
of pesticides dissolved and suspended in water. OC pesticides have a relatively short half-life in wa-
ter (<30 days), are practically insoluble in it (<50 mg/L)
The highest incidence of different types of pesticide and immobile (Koc> 4000 mL/g), and volatility per
residues in the months of July, August and September Henry’s law constant is moderate (0.1 Pa m3/mol –
concur with the end of spring-summer crop season in 100 Pa m3/mol) for aldrin, DDT and endosulfan and
Culiacan Valley and rainy season arrival. This suggests high (>100 Pa m3/mol) for heptachlor. They have
that pesticides are retained in soil –considering that ap- good affinity for organic matter, so they are deposited
plication peak is February and March (Leyva-Morales et in aquatic ecosystems sediment (Instituto Nacional
al., 2014)–, and are released and transported by runoff de Ecología y Cambio Climático [INECC], 2007; Uni-
or agricultural drains to river. Some studies have sug- versity of Hertfordshire, 2007; Yang, Lv, Shi & Jiang,
gested that DDT is associated with agricultural soil ero- 2005). These characteristics may account for their
sion, and may be settled in bodies of water in a stream low concentrations in water samples. However, owing

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
Vol. 27 No. 1 Enero-Febrero 2017 49
 ISSN 0188-6266

to their high Kow (Kow> 3) OCs tend to bioaccumulate designated "α" (CAS No. 959-98-8) and "β" (CAS
in environment and may be expected to be found in 33213-65-9), in a ratio of 70:30, and it may further
higher concentrations in sediment and fish or other contain small amounts of endosulfan sulfate and oth-
aquatic organisms. ers related chemicals (Fan, 2007). It is liposoluble,
with low water solubility (0.32 mg/L) and high solubil-
DDT and its metabolites are ubiquitous and per-
ity in most organic solvents. It has a cyclic structure,
sistent compounds that have been detected in marine
low vapor pressure (Henry's law constant of 1.48 Pa
water and sediment as well as in shrimp and clams
m3/mol), a high chemical stability, and a remarkable
in AEPL near Culiacan Valley (Galindo-Reyes et al.,
resistance to attack by microorganisms. It tends to
1992; Galindo-Reyes et al., 1999a; b). Persistence of
accumulate in fatty tissue of living organisms (Kow =
DDT may be associated with extensive use throughout
4.75), and in soil (Koc = 11 500 mL/g) and groundwa-
the world, including Culiacan Valley, for both domestic
ter (Oregon State University, 1998). Mean concentra-
and agricultural purposes (Ecobichon, 1995; Carvalho
tions of endosulfan were 0.03601 µg/L, 0.0201 µg/L
et al., 2002). Most countries prohibited its use in early
1970s owing to its persistence in environment and ac- and 0.0198 µg/L for Tamazula, Humaya and Culia-
cumulation in food chain (Bolt & Degen, 2002). Mean can rivers, respectively (table 3). In water, half-life of
concentrations of DDT were 0.051 µg/L, 0.0525 µg/L α-endosulfan is approximately one to three months
and 0.0425 µg/L for Tamazula, Humaya and Culiacan whereas that of β-endosulfan and endosulfan sulfate
rivers, respectively. Carvalho et al. (2002) attributed (a transformation product of both isomers) is more
presence and high persistence of DDT in this region than two years (Fan, 2007; United Nations Environ-
to heavy seasonal application in past and discharge of ment Programme [UNEP], 2007), which explains the
residues to irrigation water. high frequency of this pesticide in river water. Also,
its use as a commercial and domestic insecticide
Endosulfan is an insecticide-acaricide of few OCs might contribute to its presence in water. This condi-
authorized in Mexico for use in cultivation of cucum- tion is associated with water run-off and attachment to
ber, pear, melon, snuff (Nicotiana sp.), tomato, wheat soil particles. This varies from season to season and
and grapes, and in industry exclusively for plants for- year to year, depending on weather conditions includ-
mulators of pesticides (Cicoplafest, 2004). Commercial ing dry and rainy seasons (Said, El Moselhy, Rashad &
product of endosulfan is a mixture of stereoisomers, Shreadah, 2008).

Table 4.
Physicochemical characteristics of pesticides identified in water of rivers in the Culiacan valley.
Water Solubility Henry's Law c
KOC d
Kow Half-Life (days) in
Pesticide Chemical Class at 20 °C (mg/L)a Constant
(mL/g)a (Log P)a Watera
(Pa m3/mol)a
Aldrin Organochlorine 0.027 1.72 × 1001 17 500 6.5 ND
Carbaryl Carbamate 9.1 9.20 × 10–05 300 2.36 12
Carbophenothion Organophosphate 0.34 5.80 × 10–01 50 000 4.75 ND
Cyromazine Triazine 13,000 5.80 × 10–09 756b 0.069 28b
Chlorpyrifos Organophosphate 1.05 0.478 8151 4.7 29.6
DDT Organochlorine 0.006 8.43 × 10–01 151 000 6.91 28e
Diazinon Organophosphate 60 6.09 × 10 –02
609 3.69 50
Endosulfan Organochlorine 0.32 1.48 11 500 4.75 20
Ethion Organophosphate 2 3.85 × 10–02 10 000 5.07 146
Heptachlor Organochlorine 0.056 3.53 × 1002 24 000 5.44 1
Lamda Cyhalothrin Pyrethroid 0.005 2.00 × 10–02 283 707 5.5 40
Lindane Organochlorine 8.52 1.483 × 10–06 1270 3.5 28
Malathion Organophosphate 148 1.00 × 10–03 1800 2.75 6b
Methyl Parathion Organophosphate 55 8.57 × 10–03 240 3 9
Permethrin Pyrethroid 0.2 1.89 × 10–01 100 000 6.1 1
Pirimicarb Carbamate 3,100 3.30 × 10–05 388b 1.7 6

: University of Hertfordshire (2007); b: Kegley, Hill, Orme & Choi (2011); cKoc = Organic Carbon Sorption Constant; dKow = Octanol-Water Partition Coefficient; e: Oregon
a

State University (1998); ND = No Data.

Source: Author’s own elaboration.

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
50 Vol. 27 No. 1 Enero-Febrero 2017 Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
 ISSN 0188-6266

Lindane (γ-HCH) constitutes about 10% – 15% of or only in one river (e.g. ethion in Culiacan River or
technical product of hexachlorocyclohexane, and is malathion in Tamazula River) (figure 2 and table 3).
authorized in Mexico for treatment of seeds of oats, Low concentrations of chlorpyrifos and diazinon are
barley, corn, sorghum and wheat, for industrial use in explained by their short half-life in environment.
plants formulators of pesticides, for control of some
pests of livestock (mites, lice, etc.) and for urban use Pyrethroids
exclusively in health campaigns (Cicoplafest, 2004).
Lindane is strongly adsorbed to soils with high levels of Lambda cyhalothrin and permethrin were detected
organic matter, but there are indications that volatiliza- with low frequency (0.7% and 2.8%, respectively). Their
tion is an important route of dissipation under tropical water solubilities are low (0.005 mg/L and 2.0 mg/L,
conditions and high temperatures. It rapidly degrades respectively). Half-life in water is 1 day for permethrin
to tetrachlorociyclohexenes and pentachlorociyclohex- and 40 days for lambda cyhalothrin. Both compounds
anes when exposed to ultraviolet radiation (Instituto have a high Koc (Koc> 4000) and Kow (Kow> 3), and for this
Nacional de Ecología [INE], 2004). Lindane is included reason can be fixed in soil, sediment, biota and organ-
in various international conventions such as Stock- ic matter and/or move to surface waters and, also bio-
holm Convention, Rotterdam Convention and Aarhus accumulate in body fat of animals. Food chain is the
Protocol on Persistent Organic Pollutants (POPs) to main route of exposure for animals and humans (table
Convention on Long-range Transboundary Air Pollu- 4) (INECC, 2007). Lambda cyhalothrin was detected
tion (INE, 2004). Mean concentrations of lindane were only in Humaya River (at 0.0212 µg/L) and permethrin
0.0104 µg/L, 0.0041 µg/L and 0.0045 µg/L for Tama- was found only in Culiacan River (at 0.2352 µg/L). Low
zula, Humaya and Culiacan rivers, respectively and concentrations and frequencies indicate a recent ap-
hence lower than those of other OCs (table 3). plication in the area (figure 2 and table 3).

Carbamates (CBs)
Organophosphates (OPs)
Carbaryl and pirimicarb were also present although
Frequencies of detection of organophosphate pesticides with very low frequency (approximately 1% of all ana-
(OPs) in samples were, in descending order, chlorpyri- lyzed samples). Whereas solubility of carbaryl in water
fos (28.5%)> diazinon (25%)> malathion (5.6%)> ethion is low (9.1 mg/L), for pirimicarb it is high (3100 mg/L).
(1.4%)> carbophenothion (0.7%)> methyl parathion Both compounds have a low half-life in water (12 and
(0.7%) (figure 2). 6 days, respectively) and also are considered moder-
ately mobile (Koc between 75 mL/g – 500 mL/g) and
Solubility in water is low (≤50 mg/L) for car- their bioaccumulation is low (Kow< 2.7). Therefore,
bophenothion, chlorpyrifos and ethion, and moder- presence of these compounds suggests a recent ap-
ate (50 mg/L– 500 mg/L) for diazinon, malathion plication. Pirimicarb and carbaryl were detected solely
and methyl parathion. Half-life in water also varies: in Culiacan River, at concentrations of 0.1113 µg/L
<30 days for chlorpyrifos, malathion and methyl para- and 0.0772 µg/L, respectively (figure 2 and table 3);
thion, 30 – 100 days for diazinon, and 100 – 365 days agricultural use is authorized in the area for a variety
for ethion. With respect to their bioaccumulation, of crops (Cicoplafest, 2004).
methyl parathion and malathion are moderately bio-
accumulative (Kow between 2.7 and 3), while other Other pesticides
OPs are highly bioaccumulative (Kow> 3). Organic
carbon sorption constant varies, with methyl para- Cyromazine, a compound of the triazines group, was
thion being slightly mobile (Koc between 75 mL/g and detected in 1.4% of samples. Its solubility in water is
500 mL/g), diazinon and malathion moderately mobile very high (13 000 mg/L), its bioaccumulation (Kow< 2.7)
(Koc between 500 mL/g and 4000 mL/g) and carbo- and half-life in water (28 days) are low, and it is con-
phenothion, chlorpyrifos and ethion highly mobile sidered slightly mobile (Koc = 756 mg/L) (INECC 2007;
(Koc> 4000 mL/g) (table 4) (INECC, 2007; University University of Hertfordshire, 2007). Cyromazine was
of Hertfordshire, 2007). Mean concentrations of diazi- detected in Tamazula and Culiacan rivers at concen-
non were 0.0296 µg/L; 0.0211 µg/L and 0.0403 µg/L trations of 0.1177 µg/L and 0.1961 µg/L, respectively
and of chlorpyrifos were 0.0296 µg/L, 0.0163 µg/L and (table 3). Cyromazine was detected in Tamazula and
0.0157 µg/L for Tamazula, Humaya and Culiacan riv- Culiacan Rivers at 0.1177 µg/L and 0.1961 µg/L, respec-
ers, respectively. Other OPs were detected infrequently tively (table 3).

Monitoring of pesticides residues in... | José Belisario Leyva Morales, José Benigno Valdez Torres,
Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
Vol. 27 No. 1 Enero-Febrero 2017 51
 ISSN 0188-6266

Carvalho, F. P., González-Farías, F., Villeneuve, J. P., Cattini, C., Hernández-Gar-

CONCLUSIONS
za, M., Mee, L. D., & Fowler, S. W. (2002). Distribution, fate and effects of pes-
Pesticides detected in Culiacan River lower basin were ticide residues in tropical coastal lagoons of northwestern Mexico. Environ-
at concentrations below the maximum allowed by mental Technology, 23(11), 1257-1270. doi: 10.1080/09593332308618321
national (DOF, 1989) and international (EPA, 2006) Comisión Intersecretarial para el control de procesos y uso de plaguicidas, fer-
laws that enforce protection of freshwater aquatic life. tilizantes y sustancias tóxicas (Cicoplafest). (2004). Catálogo Oficial de
They indicate a low influence of agricultural activities, Plaguicidas. Mexico: Secretaría de Medio Ambiente y Recursos Natura-
as well as, proper use of agricultural pesticides in les (Semarnap) / Secretaría de Comercio y Fomento Industrial (Secofi) /
studied region. SAGAR / Secretaría de Salud (SSA).

Some compounds of recent use are not covered by Comisión Nacional del Agua (Conagua). (2004). Catálogo oficial de plaguicidas.
any of regulations (e.g. cyromazine) so it would be in- Comisión Intersecretarial para el Control del Proceso y Uso de Plaguicidas,
structive to compare their presence here with records Fertilizantes y Sustancias Tóxicas. México D.F. 483 pp.Retrieved January
from other parts of the world. 8, 2014 from http://www.cofepris.gob.mx/AZ/Paginas/Plaguicidas%20y%20
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Most of compounds found were organochlorines
indicating historical contamination, mainly associat- Darko, G., Akoto, O., & Oppong, C. (2008). Persistent organochlorine pesticide
ed with DDT metabolites not necessarily parent com- residues in fish, sediments and water from Lake Bosomtwi, Ghana. Che-
pound. Use of some of these compounds (e.g. lindane) mosphere, 72(1), 21-24. doi: 10.1016/j.chemosphere.2008.02.052
has been restricted in Mexico, whereas in some coun-
De la Lanza Espino, G., & Flores-Verdugo, F. (1998). Nutrient fluxes in sedi-
tries they have already been banned. However, compar-
ment (NH4+ and PO4-3) in NW coastal lagoon Mexico associated with an
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agroindustrial basin. Water, Air, and Soil Pollution, 107(1-4), 105-120. doi:
pesticide contamination derived from runoffs toward
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river from contaminated soil particles and not from
use of pesticides in intensive agriculture of region. Diario Oficial de la Federación (DOF). (2 de diciembre de 1989). Criterios ecológi-
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ACKNOWLEDGEMENTS 7, 2014 from http://www.dof.gob.mx/nota_detalle.php?codigo=4837548&fec
ha=13/12/1989
Authors thank at Q.F.B. Hector Carrillo Yáñez, M. Sc.
Eduardo Sánchez Valdez and L.I. Jorge Manjarrez for Ecobichon, D. J. (1995). Toxic effects of pesticides: organochlorine insecticides.
their participation in sampling activities and at Ann In C.D. Klaassen, M.O. Amdur & J. Doull (Eds.), Casarett and Doull’s Toxi-
Grant for English language revision. This study was cology: The basic science of poisons, 5, (pp. 649-655). New York, USA:
partially supported by Pesticide Toxicology Network McGraw-Hill.
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Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54
Vol. 27 No. 1 Enero-Febrero 2017 53
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54 Vol. 27 No. 1 Enero-Febrero 2017 Pedro de Jesús Bastidas Bastidas, Miguel Ángel Angulo Escalante, Juan Ignacio SarmientoSánchez,
Alma Lorena Barraza Lobo, Claudia Olmeda Rubio, Cristóbal Chaidez Quiroz | pp. 45-54