Gastrodia Elata, Dogwood, And Mistletoe In Pesticide Residue Determination Method Research

Gas chromatography methods were established for simultaneous determination of organochlorine and pyrethroid pesticide residues in Gastrodia elata Bl., Cornus officinalis Sieb.et Zucc. and Viscum coloratum (Komar.) Nakai by cloud-point extraction (CPE) and dispersive solid phase extraction (DSPE). The sample and rapid methods were applied to pesticide recidues detection and security monitoring and control.Gas chromatography method was developed for simultaneous determination of organochlorine and pyrethroid pesticide residues in Gastrodia elata Bl., Cornus officinalis Sieb.et Zucc.and Viscum coloratum (Komar.) Nakai. DB-1 capillary column (30 m×0.25 mm×0.25μm) was used. The detector was ECD. The temperature of detector was 280℃. The Inlet temperature was 230℃. The temperature of column was 150℃after injection then programmed at 5℃·min-1 to 250 for 1 min and at 2℃·min-1 to 270℃for 5 min. The calibration curves were linear over the concentraction range of 5-500μg·L-1 for organochlorine pesticides and 10-1000μg·L-1 for pyrethroid pesticides (r was in the range of 0.9978-1.0000).Cloud point extraction was used for extraction and purification to pesticide residues in Gastrodia elata Bl., Cornus officinalis Sieb.et Zucc. and Viscum coloratum (Komar.) Nakai. We optimized the surfactant, re-extractant, and the time of extraction, equilibration and re-extraction. A cloud point extraction method was established with the non-ionic surfactant Triton X-100 as the extractant,30 min as the time of extraction,15 min as the time of equilibration, n-hexane as the re-extractant and 5 min as the time of extraction. Pesticide residues of organochlorine and pyrethroid were detemined with gas chromatography. The limit of quantity is 3μg-kg-1-15μg·kg-1. In Gastrodia elata Bl., the recovery range was 77.41%-111.9%, and the range of the relative standard deviations is below 1.6%-9.2%. In Cornus officinalis Sieb.et Zucc., the recovery range was 79.10%-112.6%, and the range of the relative standard deviations is below 2.6%-9.3%. In Viscum coloratum (Komar.) Nakai, the recovery range was 75.45%-119.0%, and the range of the relative standard deviations is below 2.4%-9.7%. The simple and less pollution method can be developed for simultaneous determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicines.Dispersive solid phase extraction was used for extraction and purification to pesticide residues in Gastrodia elata Bl., Cornus officinalis Sieb.et Zucc. and Viscum coloratum (Komar.) Nakai. We optimized the extractant, the asorbent and the time of extraction and purification, and established a dispersive solid phase extraction method with extractant acetonitrile as the extractant and the primary secondary amine (PSA) as the adsorbent. Pesticide residues of organochlorine and pyrethroid was determined with gas chromatography. The limit of quantity is 4μg·kg-1 -20μg·kg-1. In Gastrodia elata Bl., the recovery range was 78.38%-119.1%, and the range of the relative standard deviations is below 3.0%-9.6%. In Cornus officinalis Sieb.et Zucc., the recovery range was 77.12%-118.3%, and the range of the relative standard deviations is below 2.4%-9.7%. In Viscum coloratum (Komar.) Nakai, the recovery range was 76.78%-116.4%, and the range of the relative standard deviations is below 2.5%-9.6%. The simple and less pollution method can be developed for simultaneous determination of organochlorine and pyrethroid pesticide residues in Chinese herbal medicines.Seventeen samples of Gastrodia elata Bl., Cornus officinalis Sieb.et Zucc.and Viscum coloratum (Komar.) Nakai were determined using the established methods. The determination result is consistent with that of the method of the Chinese Pharmacopoeia (Edition 2005). Organochlorine pesticides were detected in fifteen samples and pyrethroid pesticides were detected in six samples. According to Pesticide residues Limit Standard in the European Pharmacopoeia 6.0, the total quantity of the aldrin and the dieldrin Cornus officinalis Sieb.et Zucc from zhejiang 2 and henan exceeded the limits standard. Compared to the method of Chinese Pharmacopoeia, extraction and purification steps are simultaneous completion by loud-point extraction and dispersive solid phase extraction, which simplified the sample pre-treatment steps, reduced the consumption of organic reagents and increased the variety of pesticides detected with the direction and trends of pesticide residues analytical techniques consistent.