Determination of 19 Organochlorine Pesticide Residues in Sargassum Fusiforme by GC-MS / 中国药师

Objective:To establish a GC-MS method for determing 19 organochlorine pesticide residues in sargassum fusiforme. Methods:Nineteen organochlorine pesticide residues were simultaneously determined by GC-MS, and the established method was vali-dated. The HP-5 gas chromatography column (30 m × 0. 25 mm,0. 25 μm) was used. The column temperature was programming in-creased with initial temperature of 70℃, maintaining for 1min, then raising to 180℃ with a rate of 15℃·min-1 ,and then raised to 280℃ with a rate of 4℃·min-1 to keep 7min. The inlet temperature was 240℃. The MS detector was used with EI source at 230℃, and analysis mode was multiple reaction monitoring. Results:Sargassum fusiforme was analyzed. The separation degree of the standard and samples met the requirements. The recoveries of the organochlorine pesticides were 72%-127% except for hexachlorobenzene, and the relative standard deviation also met the requirements. The experimental results showed that the 19 organochlorine pesticides were not detected out in sargassum fusiforme. Conclusion: The method provides the technical parameters for the determination of organo-chlorine pesticide residues in sargassum fusiforme.

Determination of 666 and DDT pesticide residues in Anoectochili Roxburghii Gemma Terminalis by gas chromatography / 中草药

Objective: Determination of 666 (BHC) and DDT residues in Anoectochili Roxburghii Gemma Terminalis. Methods: Using gas chromatography (GC) for limited detecting the eight kinds of organochlorine pesticide residues, such as BHC (α-BHC, β-BHC, γ-BHC, and δ-BHC) and DDT (PP '-DDE, PP'-DDD, OP '-DDT, and PP'-DDT) in Anoectochili Roxburghii Gemma Terminalis. Results: Linear BHC and DDT standard curve were good, the correlation coefficient was 0.9988-0.9997, the average recovery rates were 95.4%-98.9%, 1%-2.98% RSD. The detection limitation was 0.0053-0.021 g/L. Result of Chinese herbal medici: β-BHC for G 0.0009mg/kg(Among them, α-BHC, γ-BHC, δ-BHC, PP'-DDE, OP'-DDT, PP'-DDD, PP'-DDT not detected) Conclusion: The method is accurate, reliable, scientific, and feasible, and has higher sensitivity and linear range, which can be used for quality control of pesticide residues in water.

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.

Níveis de pesticidas organoclorados em soro sanguíneo de pessoas expostas à doença de chagas no Brasil / Levels of hexachlorocyclorhexane (HCH) in exposed people from a Chagas' disease area in Brazil

Níveis de pesticidas organoclorados foram determinados em 51 amostras de sangue de moradores numa área onde a doença de Chagas é controlada pela pulverização das casas com hexaclorocicloexano (HCH) para eliminar insetos vetores. Foram coletadas 28 amostras de sangue de pessoas cujas casas foram tratadas com HCH (grupo 1) e 23 de moradores em casas não tratadas (grupo 2). Os resultados encontrados mostraram diferença significativa entre os dois grupos. No grupo 1, os níveis de HCH variaram de 1 a 35 mg/dl(ppb), com mediana de 10m/dl(ppb) e, no grupo 2, variaram de < 1mg/dl a 5m/dl, com mediana de 1m/dl. Foram detectados pp'DDE em 100% das amostras e Dieldrin em 43,1% das mesmas (AU).

Variação dos níveis de resíduos de pesticidas organoclorados em leite pasteurizado tipo B, distribuído na cidade de São Paulo, de 1980 a 1981 / Variation of organochloride pesticide residues levels in grade B pasteurized milk distributed in the city of Säo Paulo, from 1980 to 1981

Amostras de três marcas de leite pasteurizado tipo B, comercializadas na cidade de São Paulo, foram analisadas pelo método da cromatografia em fase gasosa com detetor de captura de elétrons, a fim de avaliar os níveis de resíduos de pesticidas organoclorados. Foram coletadas trinta e seis amostras no ano de 1980 e doze em 1981. A finalidade destas análises foi a de verificar o efeito, nos últimos anos, das medidas regulamentares de defensivos agrícolas adotadas em nosso País, sobre os resíduos de pesticidas organoclorados no leite de vaca e também comparar os novos resultados com os obtidos anteriormente, durante os anos de 1971 a 1979. Em 1980, esses valores variaram de 0,02 mg/kg a 0,70 mgykg' e de 0,00 mg/kg a 0,22 mg/kg para HCH total e somatória de DDT, respectivamente. Em 1981 a variação oscilou entre 0,10 mgv'kg a 0,33 mg/kg e 0,00 mg Zkg a 0,10 mgv'kg para HCH total e somatória de DDT, respectivamente. O gráfico das medianas apresentou valores mais altos em 1980 para HCH em relação aos de 1979 e 1981; o mesmo aconteceu para a somatória de DDT, mas apenas na amostra A, representando uma estabilização desses resíduos nas demais amostras. Das amostras analisadas em 1981, 50% revelaram níveis baixos de Dieldrin, percentagem inferior aos 72% do ano anterior. Todos os valores citados foram calculados na gordura do leite (AU).