Improvement of detection limits of flame-spectrophotometric determination of chlorinated organic pesticide residues

The Analyst ◽  
1969 ◽  
Vol 94 (1124) ◽  
pp. 1033 ◽  
Author(s):  
Roland Herrmann ◽  
Brigitte Gutsche
2003 ◽  
Vol 71 (3) ◽  
pp. 179-194
Author(s):  
W. El-Hawary ◽  
A. Shoukry ◽  
A. Talat

The interaction of hydralazine hydrochloride with picric acid (I), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) (II), 2,4-dinitrobenzoic acid (III), bromanil (IV) and chloranil (V) was found to be useful for its spectrophotometric determination. The determination was carried out at 520, 510, 550, 540 and 535 nm for the reaction with (I), (II), (III), (IV) and (V), respectively. The effect of several variables on the colouring process was studied. The proposed methods have been applied successfully for the determination of hydralazine hydrochloride in pure samples and in pharmaceutical preparations with good accuracy and precision. The results were compared to those obtained by the official and pharmacopoeia1 methods. The linear ranges for obedience of Beer's law are up to 118, 54,639, 27.5 and 78.6 mg/l, Ringbom ranges are 13-100, 7.6-44.7, 77.4-445.0, 5.8-25.8 and 22.5-63.1 μg/ml, Detection limits are 4.8, 2.2, 18.4, 1.2 and 5.9 mg/l, and RSD 0.042, 0.037, 0.043, 0.013 and 0.073 for reactions of hydralazine hydrochloride with I, II, III, IV and V, respectively.


1963 ◽  
Vol 46 (2) ◽  
pp. 182-186
Author(s):  
Martin Eidelman

Abstract The dimethyl sulfoxide procedure was extended to eleven edible oils and fish oils. After cleanup, the detection system of choice may be used. If extracts of samples larger than 20 g are injected into the microcoulometric detection system, halogenated background material will make evaluation difficult. In fish oils, when paper chromatography is used for evaluation, an Rf indicating aldrin must be further investigated, since it is possible that a spot at this Rf might be background material.


Author(s):  
MARIA TERESA PLATA OVIEDO ◽  
MARIA CECÍLIA DE FIGUEIREDO TOLEDO ◽  
EDUARDO VICENTE

Foram analisados resíduos de Clorotalonil, Aldrin, Dieldrin, Heptacloro, Heptacloro epóxido, Endosulfan alfa, Endosulfan beta e Sulfato de Endosulfan nas seguintes hortaliças: alface, acelga, chicória, repolho, tomate, chuchu, batata, cenoura, mandioca e mandioquinha. As amostras foram coletadas no restaurante da Universidade Estadual de Campinas, no período de abril/1998 a abril/ 2001 e nas Centrais de Abastecimento de Campinas, no período de abril a agosto/2001. Os resíduos dos agrotóxicos organoclorados foram determinados por cromatografia a gás com detector de captura de elétrons (CG-DCE- 63Ni). Os limites de detecção (LD) encontrados para Clorotalonil, Aldrin, Dieldrin, Heptacloro, Heptacloro epóxido, Endosulfan alfa, Endosulfan beta e Sulfato de Endosulfan foram 0,0006, 0,0006, 0,0008, 0,0006, 0,0007, 0,0008, 0,0009 e 0,0016 mg/kg, e os limites de quantificação 0,002, 0,002, 0,003, 0,002, 0,003, 0,003, 0,003 e 0,005 mg/kg, respectivamente. A recuperação média dos agrotóxicos analisados variou de 76,0 a 97,0% em repolho, de 90,0 a 103,0% em tomate e de 81,0 a 106,0% em batata. Em todas as amostras de hortaliças analisadas (n=151), os níveis residuais de agrotóxicos apresentaram-se abaixo dos limites de detecção (LD) do método validado. DETERMINATION OF ORGANOCHLORINE PESTICIDES RESIDUES ON VEGETABLES Abstract Residues of Chlorotalonil, Aldrin, Dieldrin, Heptachlor, Heptachlor epoxide, alpha and beta Endosulfan and Endosulfan sulfate were analysed in the following vegetables: lettuce, swiss chad, chicory, cabbage, tomato, chayote, potato, carrot, cassava and cassava specy. The samples were collected at the restaurant of the University of Campinas, from April/1998 to April/2001 at the “Centrais de Abastecimento de Campinas (CEASA)”, from April to August/2001. The organochlorine pesticide residues were determined by gas chromatography with an electron capture detector (ECD-63Ni). The detection limits of Chlorotalonil, Aldrin, Dieldrin, Heptachlor, Heptachlor epoxide, alpha and beta Endosulfan and Endosulfan sulfate were 0.0006, 0.0006, 0.0008, 0.0006, 0.0007, 0.0008, 0.0009 and 0.0016 mg/kg respectively, and their quantification limits were 0.002, 0.002, 0.003, 0.002, 0.003, 0.003, 0.003 and 0.005 mg/kg. The average recovery of the pesticides varied between 76.0 and 97.0% for cabbage, 90,0 to 103.0% for tomato and 81.0 to 106.0% for potato. The samples analysed (n=151) showed pesticide levels below the detection limits of the validated method.


2012 ◽  
Vol 77 (7) ◽  
pp. 911-917 ◽  
Author(s):  
Valéria Guzsvány ◽  
Sanja Lazic ◽  
Natasa Vidakovic ◽  
Zsigmond Papp

A simple first-order derivative spectrophotometric method was developed for the simultaneous determination of acetamiprid and 6-chloronicotinic acid (6-CNA) at pH 7.0. By using the zero-crossing approach, acetamiprid was determined at 269.0 nm and 6-CNA at 216.0 nm with the detection limits of 7.19x10-7 and 8.25x10-7 mol dm-3, respectively and relative standard deviations not exceeding 1.2% in the case of model systems.


2019 ◽  
Vol 79 ◽  
pp. 03013
Author(s):  
Xiao-mei Yang ◽  
Yi-peng Gu ◽  
Shu-jie Wu ◽  
Ling Feng ◽  
Fang Xie

A rapid detection method of pesticide residues in milk by enzyme inhibition was researched. Construction of a quickly reaction system of enzyme inhibition for determination of organophosphorus and carbamate pesticide residues was achieved. The analysis of color reactions of milk showed a good correlation between color intensity and content of tolclofos-methyl, methamidophos and isoprocarb 1-naphthalenyl methyl carbamate. The detection limits of the four pesticide were 0.5~1.0 mg/kg, which were below the level of detection required to satisfy legislation in china. This method is simple and inexpensive and suitable for rapid detection of pesticide residues in milk.


2018 ◽  
Author(s):  
Xhulieta Hamiti ◽  
Ilirjana Boci ◽  
Pranvera Lazo

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