Validation of a multi-residue method to determine deltamethrin and alpha-cypermethrin in mosquito nets by gas chromatography with electron capture detection (GC-μECD)

Particle and Fibre Toxicology

Pieter Spanoghe³  Olivier Pigeon¹  Jean Pierre Nabléni Ouattara² 

[1] Walloon Agricultural Research Centre (CRA-W), Agriculture and Natural Environment Department, Plant Protection and Biocides Physico-Chemistry and Residues Unit, Rue du Bordia, 11, Gembloux, B-5030, Belgium;Laboratoire National de Santé Publique (LNSP), Boulevard des Tansoba kiéma, Ouagadougou 09 09 BP 24, Burkina Faso;Department of Crop Protection, Laboratory of Crop Protection Chemistry, Ghent University, Coupure links 653, Gent B-9000, Belgium

关键词: GC-μECD;    Alpha-cypermethrin;    Deltamethrin;    Mosquito net;    Analytical method validation;   

Others  :  1228025
DOI  :  10.1186/1756-3305-6-77

 received in 2012-10-22, accepted in 2013-03-12,  发布年份 2013

【 摘 要 】

Background

Nowadays long-lasting insecticidal mosquito nets (LNs) are frequently used around the world to protect people against malaria vectors. As they contain insecticide, laboratory control is needed to check whether the content of the active ingredient follows the conditions of the manufacturer and also if the active ingredient is still present after some time of use. For this purpose, an analytical method had to be developed. The fact that LNs include a range of polymers for the yarn and use coated or incorporated technologies for the active ingredient, it is a challenge to find only one analytical method determining the active ingredient in LNs, which takes into account both impregnation technologies. Some methods are provided by international organizations but are limited by the determination of only one pesticide per method. The aim of this study was to optimize a short time extraction method for deltamethrin and alpha-cypermethrin from coated and incorporated mosquito nets and also to detect both insecticides in one analytical run, using gas chromatography with electron capture detection (GC-μECD).

Methods

Based on the literature, the most suitable solvent and the adequate extraction process for the insecticides used for net making were identified and adapted for the new multi-residue method.

Results

The validation data of the multi-residue method to determine deltamethrin and alpha-cypermethrin in mosquito nets by GC-μECD are given. Depending on the concentration of the active ingredient spiked on the nets, the mean recovery for alpha-cypermethrin ranged between 86% and 107% with a relative standard deviation below 3.5%. For deltamethrin it ranged between 90% and 108% with a relative standard deviation also below 3.5%. The limit of detection is 0.009 g.a.i/kg of net (0.3 mg a.i./m² of net) both for alpha-cypermethrin and deltamethrin.

Conclusions

Data obtained are excellent. A 30 minutes reflux extraction method with xylene was developed to determine alpha-cypermethrin and deltamethrin in long-lasting insecticidal mosquito nets (LNs) by gas chromatography with electron capture detection (GC-μECD). The method can be easily extended to others pyrethroid used for mosquito net treatment. This paper also presents an overview of the studies dealing with pesticide determination in mosquito nets.

【 授权许可】

   
2013 Ouattara et al.; licensee BioMed Central Ltd.

【 图 表 】

Figure 1.

Figure 2.

Figure 3.

【 参考文献 】

• [1]Manual on development and use of FAO and WHO specifications for pesticides. http://www.fao.org/fileadmin/templates/agphome/documents/Pests_Pesticides/PestSpecsManual.pdf webcite
• [2]ISO - International Standard Organization: General requirements for the competence of testing and calibration laboratories ISO/IEC 17025:2005. Geneva: ISO; 2005.
• [3]Collaborative International Pesticides Analytical Counci. [http://www.cipac.org/ webcite
• [4]Müller MD, Pigeon O: CIPAC Guideline for LN-methods: Work flow for integration of analytical and physical-chemical methods for ln into related CIPAC methods for corresponding active ingredients. http://www.cipac.org/document/Guidance%20Documents/CIPAC_LN__work_flow_May_09_final_090526.pdf webcite
• [5]CIPAC - Collaborative International Pesticides Analytical Council: Permethrin Long lasting insecticidal net (331/LN/M/-). England: CIPAC Methods and Publications; 2007.
• [6]CIPAC - Collaborative International Pesticides Analytical Council: Deltamethrin Long lasting insecticidal nets (333/LN/(M)/-). England: CIPAC Methods and Publications; 2007.
• [7]CIPAC - Collaborative International Pesticides Analytical Council: Deltamethrin Long lasting insecticidal nets (333/LN/(M2)/-). England: CIPAC Methods and Publications; 2009.
• [8]CIPAC - Collaborative International Pesticides Analytical Council: Alpha-Cypermethrin Insecticidal nets (454/LN/M/-). England: CIPAC Methods and Publications; 2007.
• [9]Hassan V, Hossein M, Mansoreh S, Reza AM, Reza YEM, Ahmad R, Mohammad A, Fatemeh R, Fatemeh N: Evaluation of bioefficacy of alpha -cypermethrin in long lasting impregnated net (Interceptor (R)) using analytical method. Asian Pacific Journal of Tropical Medicine 2010, 3:642-646.
• [10]Kilian A, Byamukama W, Pigeon O, Atieli F, Duchon S, Phan C: Long-term field performance of a polyester-based long-lasting insecticidal mosquito net in rural Uganda. Malar J 2008, 7:1-22. BioMed Central Full Text
• [11]Hemingway RJ: IUPAC Reports on pesticides (18) Improved cost-effective approaches to pesticide residues analysis. Pure and Applied Chemistry 1984, 56:1131-1152.
• [12]APVMA - Australian Pesticides and Veterinary Medicines Authority: Guidelines for the validation of analytical methods for active constituent, agricultural and veterinary chemical products. 2004. http://www.apvma.gov.au/publications/guidelines/docs/gl_69_analytical_methods.pdf webcite
• [13]CIPAC - Collaborative International Pesticides Analytical Council: Guidelines on method validation to be performed in support of analytical methods for agrochemical formulations. http://www.cipac.org/document/guidance%20documents/validat.pdf webcite
• [14]Green JM: A practical guide to analytical method validation. Anal Chem 1996, 68:A305-A309.
• [15]Miller JN, Ambrus A: Chapter 9: Statistics in calibration analysis (I). In Manual on Basic Statistics. FAO/IAEA Training and Reference Centre for Food and Pesticide Control Vienna: Australia; 2000.
• [16]CEAEQ - Centre d’expertise en analyse environnementale du Québec: Protocole pour la validation d'une méthode d'analyse en chimie. 2009. http://www.ceaeq.gouv.qc.ca/accreditation/pala/dr12vmc_protocole_val_chimie.pdf webcite
• [17]Pigeon O, Ducat N: Determination of alpha cypermethrin in Long - Lasting (coated onto polyester or incorporated into polyethylene) Insecticidal Mosquito Nets (coated or incorporated LNs) Method by GC-FID. In Method N° ResSM016 - version 6. Gembloux: Plant Protection Products and Biocides Physico-chemistry and residues Unit: Walloon Agricultural Research Centre (CRA-W); 2010. Unpublished
• [18]Kilian A, Byamukama W, Pigeon O, Gimnig J, Atieli F, Koekemoer L, Protopopoff N: Evidence for a useful life of more than three years for a polyester-based long-lasting insecticidal mosquito net in Western Uganda. Malar J 2011, 10:1-13. BioMed Central Full Text
• [19]Banek K, Kilian A, Allan R: Evaluation of Interceptor long-lasting insecticidal nets in eight communities in Liberia. Malar J 2010, 9:1-11. BioMed Central Full Text
• [20]Kayedi MH, Kaur H, Haghdoost AA, Lines JD: The effects of different drying methods and sun exposure on the concentrations of deltamethrin in nets treated with K-O Tab (R) tablets. Ann Trop Med Parasitol 2009, 103:85-90.
• [21]Graham K, Kayedi MH, Maxwell C, Kaur H, Rehman H, Malima R, Curtis CF, Lines JD, Rowland MW: Multi-country field trials comparing wash-resistance of PermaNet (TM) and conventional insecticide-treated nets against anopheline and culicine mosquitoes. Medical and Veterinary Entomology 2005, 19:72-83.
• [22]Yates A, N'Guessan R, Kaur H, Akogbeto M, Rowland M: Evaluation of KO-Tab 1-2-3 (R): a wash-resistant 'dip-it-yourself' insecticide formulation for long-lasting treatment of mosquito nets. Malar J 2005, 4:1-9. BioMed Central Full Text
• [23]Oxborough RM, Weir V, Irish S, Kaur H, N'Guessan R, Boko P, Odjo A, Metonnou C, Yates A, Akogbeto M, Rowland MW: Is K-O Tab 1-2-3 (R) long lasting on non-polyester mosquito nets? Acta Trop 2009, 112:49-53.
• [24]Jones CM, Sanou A, Guelbeogo WM, Sagnon N, Johnson PCD, Ranson H: Aging partially restores the efficacy of malaria vector control in insecticide-resistant populations of Anopheles gambiae s.l. from Burkina Faso. Malar J 2012, 11:1-11. BioMed Central Full Text
• [25]Pigeon O, Ducat N: Determination of deltamethrin in Long-Lasting (coated onto polyester) Insecticidal Mosquito Nets (coated LNs) Method by HPLC-DAD or GC-FID. In Method N° ResSM014 - version 3. Gembloux: Plant Protection Products and Biocides Physico-chemistry and residues Unit, Walloon Agricultural Research Centre (CRA-W); 2010. Unpublished
• [26]Corbel V, Chabi J, Dabire RK, Etang J, Nwane P, Pigeon O, Akogbeto M, Hougard JM: Field efficacy of a new mosaic long-lasting mosquito net (PermaNet (R) 3.0) against pyrethroid-resistant malaria vectors: a multi centre study in Western and Central Africa. Malar J 2010, 9:1-12. BioMed Central Full Text
• [27]Tungu P, Magesa S, Maxwell C, Malima R, Masue D, Sudi W, Myamba J, Pigeon O, Rowland M: Evaluation of PermaNet 3.0 a deltamethrin-PBO combination net against Anopheles gambiae and pyrethroid resistant Culex quinquefasciatus mosquitoes: an experimental hut trial in Tanzania. Malar J 2010, 9:1-13. BioMed Central Full Text
• [28]Pigeon O, Rousseau G: Determination of deltamethrin and/or piperonyl butoxide in Long-Lasting (incorporated into polyethylene) Insecticidal Mosquito Nets (incorporated LNs)Method by GC-FID. In Method N° ResSM015 - version 3. Gembloux: Plant Protection Products and Biocides Physico-chemistry and residues Unit, Walloon Agricultural Research Centre (CRA-W); 2009. Unpublished
• [29]Pigeon O, Vandecandelaere S, Vandenberghe J-P, Hérion V, Demeulenaere J-L, Wellin A, Laduron L, Boinon N: Determination of deltamethrin and PBO in (incorporated into polyethylene) LN. In In the 53rd Collaborative International Pesticides Analytical Council Symposium: 10 June 2009. Hotel Decameron Salinitas, El Salvador: CIPAC; 2009.
• [30]Muller O, Ido K, Traore C: Evaluation of a prototype long-lasting insecticide-treated mosquito net under field conditions in rural Burkina Faso. Transactions of the Royal Society of Tropical Medicine and Hygiene 2002, 96:483-484.
• [31]Skovmand O, Bonnet J, Pigeon O, Corbel V: Median knock-down time as a new method for evaluating insecticide-treated textiles for mosquito control. Malar J 2008, 7:1-8. BioMed Central Full Text
• [32]Gimnig JE, Lindblade KA, Mount DL, Atieli FK, Crawford S, Wolkon A, Hawley WA, Dotson EM: Laboratory wash resistance of long-lasting insecticidal nets. Tropical Medicine & International Health 2005, 10:1022-1029.
• [33]Lindblade KA, Dotson E, Hawley WA, Bayoh N, Williamson J, Mount D, Olang G, Vulule J, Slutsker L, Gimnig J: Evaluation of long-lasting insecticidal nets after 2 years of household use. Tropical Medicine & International Health 2005, 10:1141-1150.
• [34]Faulde M, Albiez G, Nehring O: Novel long-lasting impregnation technique transferred from clothing to bednets: extended efficacy and residual activity of different pyrethroids against Aedes aegypti as shown by EN ISO 6330-standardized machine laundering. Parasitol Res 2012, 110:2341-2350.
• [35]Faulde MK, Albiez G, Nehring O: Insecticidal, acaricidal and repellent effects of DEET- and IR3535-impregnated bed nets using a novel long-lasting polymer-coating technique. Parasitol Res 2010, 106:957-965.
• [36]CIPAC - Collaborative International Pesticides Analytical Council: Lambda-cyhalothrin long lasting insecticidal nets (463/LN/M/-). England: CIPAC Methods and Publications; 2010.
• [37]CIPAC - Collaborative International Pesticides Analytical Council: Piperonyl butoxide Long lasting insecticidal nets. England: CIPAC Methods and Publications; 2009.
• [38]WHO - World Health Organization: Insecticide-treated mosquito nets: a WHO position statement. Geneva: WHO Global Malaria Programme; 2007.
• [39]Rafinejada J, Vatandoosta H, Nikpoora F, Abaia MR, Shaeghia M, Duchenb S, Rafia F: Effect of washing on the bioefficacy of insecticide-treated nets (ITNs) and long-lasting insecticidal nets (LLINs) against main malaria vector Anopheles stephensi by three bioassay methods. Journal of vector borne diseases 2008, 45:143-150.