Honey as a bioindicator of environmental organochlorine insecticides contamination / Mel como bioindicador de contaminação ambiental de inseticidas organoclorados

Abstract Honey is a suitable matrix for the evaluation of environmental contaminants including organochlorine insecticides. The present study was conducted to evaluate residues of fifteen organochlorine insecticides in honey samples of unifloral and multifloral origins from Dir, Pakistan. Honey samples (5 g each) were extracted with GC grade organic solvents and then subjected to Rotary Evaporator till dryness. The extracts were then mixed with n-Hexane (5 ml) and purified through Column Chromatography. Purified extracts (1μl each) were processed through Gas Chromatograph coupled with Electron Capture Detector (GC-ECD) for identification and quantification of the insecticides. Of the 15 insecticides tested, 46.7% were detected while 53.3% were not detected in the honey samples. Heptachlor was the most prevalent insecticide with a mean level of 0.0018 mg/kg detected in 80% of the samples followed by β-HCH with a mean level of 0.0016 mg/kg detected in 71.4% of the honey samples. Honey samples from Acacia modesta Wall. were 100% positive for Heptachlor with a mean level of 0.0048 mg/kg followed by β-HCH with a mean level of 0.003 mg/kg and frequency of 83.3%. Minimum levels of the tested insecticides were detected in the unifloral honey from Ziziphus jujuba Mill. Methoxychlor, Endosulfan, Endrin and metabolites of DDT were not detected in the studied honey samples. Some of the tested insecticides are banned in Pakistan but are still detected in honey samples indicating their use in the study area. The detected levels of all insecticides were below the Maximum Residue Levels (MRLs) and safe for consumers. However, the levels detected can cause mortality in insect fauna. The use of banned insecticides is one of the main factors responsible for the declining populations of important insect pollinators including honeybees.

Resumo O mel é uma matriz adequada para a avaliação de contaminantes ambientais, incluindo inseticidas organoclorados. O presente estudo foi conduzido para avaliar resíduos de 15 inseticidas organoclorados em amostras de mel de origem unifloral e multifloral de Dir, Paquistão. Amostras de mel (5 g cada) foram extraídas com solventes orgânicos de grau GC e, em seguida, submetidas ao evaporador rotativo até a secura. Os extratos foram então misturados com n-hexano (5 ml) e purificados por cromatografia em coluna. Os extratos purificados (1μl cada) foram processados através de cromatógrafo gasoso acoplado a detector de captura de elétrons (GC-ECD) para identificação e quantificação dos inseticidas. Dos 15 inseticidas testados, 46,7% foram detectados enquanto 53,3% não foram detectados nas amostras de mel. O heptacloro foi o inseticida mais prevalente com um nível médio de 0,0018 mg / kg detectado em 80% das amostras, seguido por β-HCH com um nível médio de 0,0016 mg / kg detectado em 71,4% das amostras de mel. Amostras de mel da parede de Acacia modesta foram 100% positivos para heptacloro com um nível médio de 0,0048 mg / kg seguido por β-HCH com um nível médio de 0,003 mg / kg e frequência de 83,3%. Níveis mínimos dos inseticidas testados foram detectados no mel unifloral de Ziziphus jujuba da usina. Metoxicloro, Endosulfan, Endrin e metabólitos do DDT não foram detectados nas amostras de mel estudadas. Alguns dos inseticidas testados são proibidos no Paquistão, mas ainda são detectados em amostras de mel, indicando seu uso na área de estudo. Os níveis detectados de todos os inseticidas estavam abaixo dos Níveis Máximos de Resíduos (MRLs) e seguros para os consumidores. No entanto, os níveis detectados podem causar mortalidade na fauna de insetos. O uso de inseticidas proibidos é um dos principais fatores responsáveis pelo declínio das populações de importantes insetos polinizadores, incluindo as abelhas.

Honey as a bioindicator of environmental organochlorine insecticides contamination / Mel como bioindicador de contaminação ambiental de inseticidas organoclorados

Honey is a suitable matrix for the evaluation of environmental contaminants including organochlorine insecticides. The present study was conducted to evaluate residues of fifteen organochlorine insecticides in honey samples of unifloral and multifloral origins from Dir, Pakistan. Honey samples (5 g each) were extracted with GC grade organic solvents and then subjected to Rotary Evaporator till dryness. The extracts were then mixed with n-Hexane (5 ml) and purified through Column Chromatography. Purified extracts (1μl each) were processed through Gas Chromatograph coupled with Electron Capture Detector (GC-ECD) for identification and quantification of the insecticides. Of the 15 insecticides tested, 46.7% were detected while 53.3% were not detected in the honey samples. Heptachlor was the most prevalent insecticide with a mean level of 0.0018 mg/kg detected in 80% of the samples followed by β-HCH with a mean level of 0.0016 mg/kg detected in 71.4% of the honey samples. Honey samples from Acacia modesta Wall. were 100% positive for Heptachlor with a mean level of 0.0048 mg/kg followed by β-HCH with a mean level of 0.003 mg/kg and frequency of 83.3%. Minimum levels of the tested insecticides were detected in the unifloral honey from Ziziphus jujuba Mill. Methoxychlor, Endosulfan, Endrin and metabolites of DDT were not detected in the studied honey samples. Some of the tested insecticides are banned in Pakistan but are still detected in honey samples indicating their use in the study area. The detected levels of all insecticides were below the Maximum Residue Levels (MRLs) and safe for consumers. However, the levels detected can cause mortality in insect fauna. The use of banned insecticides is one of the main factors responsible for the declining populations of important insect pollinators including honeybees.

O mel é uma matriz adequada para a avaliação de contaminantes ambientais, incluindo inseticidas organoclorados. O presente estudo foi conduzido para avaliar resíduos de 15 inseticidas organoclorados em amostras de mel de origem unifloral e multifloral de Dir, Paquistão. Amostras de mel (5 g cada) foram extraídas com solventes orgânicos de grau GC e, em seguida, submetidas ao evaporador rotativo até a secura. Os extratos foram então misturados com n-hexano (5 ml) e purificados por cromatografia em coluna. Os extratos purificados (1μl cada) foram processados através de cromatógrafo gasoso acoplado a detector de captura de elétrons (GC-ECD) para identificação e quantificação dos inseticidas. Dos 15 inseticidas testados, 46,7% foram detectados enquanto 53,3% não foram detectados nas amostras de mel. O heptacloro foi o inseticida mais prevalente com um nível médio de 0,0018 mg / kg detectado em 80% das amostras, seguido por β-HCH com um nível médio de 0,0016 mg / kg detectado em 71,4% das amostras de mel. Amostras de mel da parede de Acacia modesta foram 100% positivos para heptacloro com um nível médio de 0,0048 mg / kg seguido por β-HCH com um nível médio de 0,003 mg / kg e frequência de 83,3%. Níveis mínimos dos inseticidas testados foram detectados no mel unifloral de Ziziphus jujuba da usina. Metoxicloro, Endosulfan, Endrin e metabólitos do DDT não foram detectados nas amostras de mel estudadas. Alguns dos inseticidas testados são proibidos no Paquistão, mas ainda são detectados em amostras de mel, indicando seu uso na área de estudo. Os níveis detectados de todos os inseticidas estavam abaixo dos Níveis Máximos de Resíduos (MRLs) e seguros para os consumidores. No entanto, os níveis detectados podem causar mortalidade na fauna de insetos. O uso de inseticidas proibidos é um dos principais fatores responsáveis pelo declínio das populações de importantes insetos polinizadores, incluindo as abelhas.

Honey as a bioindicator of environmental organochlorine insecticides contamination

Abstract Honey is a suitable matrix for the evaluation of environmental contaminants including organochlorine insecticides. The present study was conducted to evaluate residues of fifteen organochlorine insecticides in honey samples of unifloral and multifloral origins from Dir, Pakistan. Honey samples (5 g each) were extracted with GC grade organic solvents and then subjected to Rotary Evaporator till dryness. The extracts were then mixed with n-Hexane (5 ml) and purified through Column Chromatography. Purified extracts (1l each) were processed through Gas Chromatograph coupled with Electron Capture Detector (GC-ECD) for identification and quantification of the insecticides. Of the 15 insecticides tested, 46.7% were detected while 53.3% were not detected in the honey samples. Heptachlor was the most prevalent insecticide with a mean level of 0.0018 mg/kg detected in 80% of the samples followed by -HCH with a mean level of 0.0016 mg/kg detected in 71.4% of the honey samples. Honey samples from Acacia modesta Wall. were 100% positive for Heptachlor with a mean level of 0.0048 mg/kg followed by -HCH with a mean level of 0.003 mg/kg and frequency of 83.3%. Minimum levels of the tested insecticides were detected in the unifloral honey from Ziziphus jujuba Mill. Methoxychlor, Endosulfan, Endrin and metabolites of DDT were not detected in the studied honey samples. Some of the tested insecticides are banned in Pakistan but are still detected in honey samples indicating their use in the study area. The detected levels of all insecticides were below the Maximum Residue Levels (MRLs) and safe for consumers. However, the levels detected can cause mortality in insect fauna. The use of banned insecticides is one of the main factors responsible for the declining populations of important insect pollinators including honeybees.

Resumo O mel é uma matriz adequada para a avaliação de contaminantes ambientais, incluindo inseticidas organoclorados. O presente estudo foi conduzido para avaliar resíduos de 15 inseticidas organoclorados em amostras de mel de origem unifloral e multifloral de Dir, Paquistão. Amostras de mel (5 g cada) foram extraídas com solventes orgânicos de grau GC e, em seguida, submetidas ao evaporador rotativo até a secura. Os extratos foram então misturados com n-hexano (5 ml) e purificados por cromatografia em coluna. Os extratos purificados (1l cada) foram processados através de cromatógrafo gasoso acoplado a detector de captura de elétrons (GC-ECD) para identificação e quantificação dos inseticidas. Dos 15 inseticidas testados, 46,7% foram detectados enquanto 53,3% não foram detectados nas amostras de mel. O heptacloro foi o inseticida mais prevalente com um nível médio de 0,0018 mg / kg detectado em 80% das amostras, seguido por -HCH com um nível médio de 0,0016 mg / kg detectado em 71,4% das amostras de mel. Amostras de mel da parede de Acacia modesta foram 100% positivos para heptacloro com um nível médio de 0,0048 mg / kg seguido por -HCH com um nível médio de 0,003 mg / kg e frequência de 83,3%. Níveis mínimos dos inseticidas testados foram detectados no mel unifloral de Ziziphus jujuba da usina. Metoxicloro, Endosulfan, Endrin e metabólitos do DDT não foram detectados nas amostras de mel estudadas. Alguns dos inseticidas testados são proibidos no Paquistão, mas ainda são detectados em amostras de mel, indicando seu uso na área de estudo. Os níveis detectados de todos os inseticidas estavam abaixo dos Níveis Máximos de Resíduos (MRLs) e seguros para os consumidores. No entanto, os níveis detectados podem causar mortalidade na fauna de insetos. O uso de inseticidas proibidos é um dos principais fatores responsáveis pelo declínio das populações de importantes insetos polinizadores, incluindo as abelhas.

Determinação de bisfenol A (BFA) em água mineral por meio de CG/DCE - uma nova proposta de metodologia para análise / Bisphenol A (BPA) determination in mineral water by using CG/DCE - a new analysis methodology proposal

Neste trabalho foi avaliada a metodologia para determinar bisfenol A (BFA) em água mineral, utilizando-se a extração em fase sólida (SPE), a derivação com anidrido trifluoroacético (TFAA) e a análise por cromatografia em fase gasosa com detector de captura de elétrons (GC/ECD). A curva analítica forneceu coeficiente de correlação (R) de 0,999, valores de recuperação entre 88 e 106 por cento, limites de detecção e de quantificação de 2,5 e 25,0 ng. mL, respectivamente. A metodologia foi aplicada em quatro amostras de diferentes marcas de água mineral, dentre as quais apenas uma apresentou resultado detectável de 0,46 ng. mL. Este estudo sugere que o FBA pode ser facilmente detectado e quantificado na matriz utilizada por meio de metodologia proposta, a qual demonstrou ser seletiva, precisa e exata.

Determination of 20 organochlorine pesticide residues in Gancaoxin Granule and Fuxin Tablet by GC-ECD and GC-MS respectively and comparisons between the two methods / 中成药

AIM:To investigate the differences between GC-ECD and GC-MS methods which were employed in the determination of 20 organochlorine pesticide residues in Gancaoxin Granule(Radix et Rhizoma glycyrrhizae,zine preparation) and Fuxin Tablet(Folium Crataegi). METHODS: The solid-phase extraction was used for the clean-up of samples,the quartz capillary columns of DB-1701_(MS) and HP-5_(MS) were selected for the separations of target pesticides,ECD and MS were introduced as the detections respectively.N_2(99.99%,ECD) and He_2((99.999%,)MS) were used as carries,a column flow was at 1.0 mL/min,splitless was chosen as injection mode,injection amount was 1 ?L for all instances,the inlet was set at 230 ℃ and ECD at 300 ℃,negative ions-chemical ionization was used as ion source in MS,the source temperature was set at 200 ℃,the electron energy was at 100 eV,and the temperature of transfer line was at 290 ℃;methane was used as reagent gas with a flow of 3.0 mL/min,scan mode was for qualification,SIM mode was for quantitation. RESULTS: Because 20 organochlorine pesticides were impossible to be separated all on single column by an optimal temperature program to present maximum 19 peaks,on HP and column,both heptachlor-epoxide and oxy-chlordane appeared as a peak,while the overlaid peak in DB-1701 column was contributed by eicher pentachlorothioanisole and aldrin in ECD or oxy-chlordane and ?-666 in MS.We selected SIM mode in MS detection with different m/z and abundance to quantify.By a comparison,the residues of 20 organochlorine pesticides in two preparations showed higher in ECD than that in MS,except for hexachlorobenxene,trans-chlordane,pp'-DDE and endrin,the LOQs of 20 insecticides in ECD was commonly lower than that in MS. CONCLUSION: The ECD method has an advantage in sensitivity and precision,but its result on either qualification and quantitation is prone to the interferences of false positive peaks and background;while MS detection has high specificity in qualification and good accuracy in quantitation,but lower sensitivity and precision compared to ECD.Therefore,GC-ECD method for 20 organochlorine pesticide residues is sensitive and of good precision,while GC-MS method is rapid and accurate.

Analysis of the cyanide in biological samples by using HS / 中国法医学杂志

Objective to establish a method used for qualitative and quantitative determination of the cyanide in biological samples by using HS/GC/ECD. Method C1CN was formed as the choramines-T derivative through reaction of the potassium cyanide with chloramines-T and then was analyzed by GC/ ECD/HS. Results if 0.2ug potassium cyanide was added to 1ml blood sample, the recovery was 84.6% and RSD was 6.39%. If 0.5ug potassium cyanide was added to 1. 0g liver, the recovery was 67.3 % and RSD was 5.05%. The detection limit of blood sample was 5ng/ml. Conclusion This method can be used for analyzing the cyanide in biological samples quantitatively.