| Objective: To study the effects of new techniques for controlling Huanglong disease on the medicinal and edible quality of sugar orange fruits and the properties of ecological soil,and to show whether this control technology had an impact on the quality of sugar orange fruits as medicinal and edible.Methods: 1.Optimized the extract methods of Dichlorvos,Ethopropho,Phorate,Dimethoate,Lego,methylParathion,Chlorpyrifos,Parathion,Fenthion,Methylphofolan and Phofolan,GC spectrum was established for the determination of pesticide residues in Sugar Orange and its ecological environment soil.Acetonitrile was used to extract pesticide residues by ultrasound.Fruit samples did not need to be purified by column,but soil samples were purified by Florida silica column.2.Optimized the extract methods of heavy metal residues as Pb,Cd,Cr,As and Hg,and ICP-MS was developed for the determination of five heavy metal residues in Sugar Orange and its ecological environment soil.The microwave digestion method was used for the samples.Fruit samples were microwave digested with 8 mL nitric acid and 2 mL hydrogen peroxide,and soil samples were microwave digested with 9 mL nitric acid,2 mL hydrogen peroxide and 4 mL hydrofluoric acid.3.A plate counting method was used for the determination of total number of bacterial colonies in ecological environment soil.4.Discussed the reproducibility of extraction technology of hesperidin from Peel with reference to Pharmacopoeia,and HPLC method was used to determine its content in the peel of suger orange.The soxhlet extracted method was used to extract.Volatile oil and other interfering substances such as ultraviolet absorption were removed by petroleum ether,and then hesperidin was extracted by methanol reflux.Results: 1.Determination of organophosphorus pesticide residues in Sugar Orange and its ecological environment soil by GC with detection limit of 0.0003~0.003 mg/kg,the linear correlation coefficient were ≥ 0.9990,the recoveries of standard solution added at high,medium and low concentrations were 85.13~109.3%,and the relative standard deviation was 0.08~2.98%.This method was applied to sample analysis.Organophosphorus pesticides were not detected in fruit samples.Except for Chlorpyrifos and Dimethoate,other eight organophosphorus pesticides were not detected in the soil sample.ICP-MS was used to determinate Pb,Cr,Cd,As and Hg five heavy metal residues in Sugar Orange and its ecological environment soil.The detection limit of this method was 0.0003~0.003 mg/kg,and the linear correlation coefficient was ≥ 0.9978.The recovery rates of standard solution added in high,medium and low concentrations were 80.70~107.4%,and the relative standard deviation was 0.38~3.0%.The method was fitted to apply to analysis the samples.The results through comparative analysis,it was found that the content of heavy metals in Sugar Orange and its ecological environment soil samples under the new Huanglong disease control would not exceed the national standard limit.3.Plate counting method was used to determinate the total number of bacterial colonies in the ecological environment soil of Sugar Orange,the total number of bacterial colonies in the ecological environment soil was not shown sigificently different levels of prevention and treatment in the same orchard.4.The hesperidin in suger oranger peel was determined by HPLC,the content of hesperidin in Suger Oranger peel was not less than 3.5%,which accorded with the requirement of Pharmacopoeia that the content of hesperidin in orange peel was not less than 3.5%.Conclusions: The extraction methods for pesticides,heavy metal,and hesperidin were sufficient,efficient,simple and easy extraction,which fitted the extraction levels.The established GC method for the determination of organophosphorus pesticide residues in Sugar Orange and its ecological environment soil was simple in operation.The practical application results was good,the detection limit was very low,the recovery was good.This method could be used in determination of organophosphorus pesticide residues in fruits and soil.The established ICP-MS method for determination of heavy metal residues in Sugar Orange and its ecological environment soil was less time,and possessed widely linear range and highly sensitivity.It could detect many elements at the same time,and it was more suitable for the detection of element in fruit and soil.The established plate bacterial counting method to determine the total number of colonies in the soil was simple and efficient.Determination of hesperidin in Sugar Orange peel by HPLC with reference to pharmacopoeia was also suitable for this experimental study.The experimental results showed that: the organophosphorus pesticide residues in the new control Huanglong disease accorded with the relevant provisions of the national food safety standard GB 2763-2016.The new Huanglong disease control technology used in citrus fruits as residues of heavy metals for both medicine and food conformed to the relevant provisions of the national food safety standard GB 2762-2017.The content of hesperidin in peel was more than or equal to 3.5%,which met the limit requirement for the determination of hesperidin in orange peel of Chinese Pharmacopoeia.As for environmental pollution,after the new control Huanglong disease,organophosphorus pesticide residues in soil of ecological environment were within the scope of food-grade standards.The residues of heavy metals in soil conform to the relevant provisions of the national soil environmental quality standard GB 15618-1995.There was no significant difference in the total number of colony in soil.Therefore,the new huanglong disease control technology had no effect on the edible quality of sugar orange medicines.It could be popularized and applied to protect the interests of fruit farmers. |