| ObjectiveTo establish a gas chromatography-mass spectrometry(GC-MS) method for simultaneous determination of 38 pesticides in Chrysanthemum indicum. And pesticides residues of two bases in Hubei in the whole growth period and herbs collected from different pharmacies in Guangdong have been determined to estimate the contamination status in the region. Meanwhile, the content of total flavonoids,linarin, luteolin and chlorogenic acid in Chrysanthemum in th growth period have been detected to analysis the dynamic changes of its main components, and to provide reference for better development and utilization of chrysanthemum indicum resources.Methods and resultsThe pretreatment of multi-residuces such as sampling extraction,clean up and the parameters of GC-MS have been optimized,and the samples were using the acetonitrile as the extraction solvent and selected TPH SPE for clean-up.The experiments were performed on a DB-1701 capillary column(30mx0.25mmx0.25μm) with a temperature programming which is initial temperature 40℃ for 1 minute,then heating to 160℃ by the rate of 30℃ /min,then to 250℃ by 3℃/min, finally to 300℃ by 10℃ for 10mins. The inlet temperature was 290℃,column flow 1.0mL/min,splitless injection with inpouring 1μL.The mass speetrum was reeorded using El source,with electron energy at70eV,in selected ion monitoring mode,transmission line temperature at 280℃,ion source temperature at 230℃,quadruple temperature at 150℃. The result of the method validation suggests that the method is simple,quick and low price,and suitable for detecting pesticide multi-residues in the medicine.The extraction and the purification condition of detecting the total flavonoids were as follows:80% ethanol refluxed for 3h,by using the AB-8 type macropoious resin,after 90min, washed with water first,then with 80% alcohol as the eluant and 4 times as the eluant volume,the eluant velocity as 2～3mL/min.The method is accurate and repeatable.And it was used for the detection of the total flavonoids in different parts of Chrysanthemum in th growth period. The results showed that the total flavonoid content of the leaves in the reproductive growth stage was similar to that of the total flavonoids in flowers in the flowering stage, which could provide the raw materials for the research and application of the total flavonoids in chrysanthemum.Meanwhile,a HPLC method for simultaneous determination of linarin, luteolin and chlorogenic acid in Chrysanthemum was established,which was used for detection of 3 contents in different parts of chrysanthemum in th growth period.The results showed that the content of chlorogenic acid in leaves was the highest in vegetative growth stage,while that of root was the highest during the period of reproductive growth and flowering period. During vegetative growth period, the trend of the content of Luteolin in different parts has the following law:leaves> stems> roots;in the flowering stage, leaves> stems (roots), and the content in the leaves were extra high. The content of linarin in three periods are quite different, high content were detected in whole plant both in the vegetative growth stage and reproductive growth, and the content in the leaves was even higher than that in flowering flower. The method was applied to the determination of the pestieides in chrysanthemum in bases of Hubei,the results showed that detection rate was in 21.05%～23.68%, but all pesticide residues were lower than 0.09mg/kg. The trend of the residual of tetradifon in three periods has the following law:roots> leaves> stems; the residual of phosmet in blooming flower period:leaves> roots> flowers; and fenthion in nutrition growth stage and blooming flower stage:leaves> roots (stems),but in the reproductive growth stage:roots> leaves(stems). The trend of the residual of fenthion in the same place:in nutrition growth stage>in blooming flower period> in the reproductive growth stage; the residual of phosmet:in blooming flower period> in nutrition growth stage> in the reproductive growth stage. Also, the method was applied to the determination of the pestieides in chrysanthemum collected from real samples in Guandong, detection rate of the total BHC tetradifon, acephate, fenthion, fenvalerate pesticides in 38 kinds of pesticide residues were higher, only the content of total BHC was over the MRLConclusionA preliminary understanding of the trend of the main components in whole periods of different parts in chrysanthemum was obtained.The content of chlorogenic acid in leaves in the nutrition growth stage and that in roots in reproductive growth period were confirmed higher than tthat in flowers of blooming flower stage Since flavonoids are natural pharmaceutical active ingredients widespread in nature,which with anti-bacterial, anti-oxidant, anti-inflammatory analgesic and other biological activity.The content of total flavonoids in nutrition growth stage and reproductive growth period was similar to that in blooming flower stage, the development and utilization of chrysanthemum can not be limited to flowers, the leaves and roots in the period of vegetative growth and reproductive growth can also provide research value.A multiresidue pesticide analysis method was developed and validated for 38 pesticide in chrysanthemum combined with solid-phase extraction and gas chromatography-mass spectrometry. The method was applied to the determination of the pestieides in chrysanthemum in bases of Hubei,the results showed that detection rate was in 21.05%～23.68%, but no pesticide residues are exceeding the standard.And for the pestieides in chrysanthemum collected from real samples in Guandong, the detection rate of chlorinated pesticides are higher,but only the content of total BHC was over the MRL. Although the BHC has being banned, but metabolism of organochlorine pesticides are slow, it still be needed to focus on monitoring the residual amount. |
PDF Full Text Request