Chinese herbal medicine residual organochlorine insecticide detection method

Abstract

The present invention provides a method for examining residual organochlorine pesticides in Chinese traditional medicine, including steps of: (1) preparing a certain concentration standard solution containing nine organochlorine pesticides; (2) examining standard solution under the propriety chromatogram conditions to obtain standard chromatogram graph; (3) preparing specimen: dipping specimen powder in acetone, ultrasonic extracting by petroleum ether, purifying with sulfuric acid, decompressing and concentrating; (4) examining specimen under the same chromatogram conditions of reference substance to obtain chromatogram graph of specimen; (5) comparing the chromatogram graph between specimen and reference substance by preservation time contrast method to determine corresponding characteristic peak to calculate content by external standard method. The present method has the merits of simple operation, less disturb to tested specimen, stable data result, no damage to examining device, high recovery rate and precision, and good system reproducibility and applicability.

Description

(1) Technical field: [0001] The invention relates to a detection method, in particular to a detection method for residual organochlorine pesticides in Chinese herbal medicines. (two) background technology: [0002] Organochlorine pesticides have significant insecticidal effects and were once the most used pesticides in various countries. my country produced and used organochlorine pesticides in large quantities from the 1950s to the 1980s. Organochlorine pesticides have a long degradation period and can be enriched through the food chain. Their residual toxicity will pollute the environment and endanger human health and food safety. [0003] Plant-based Chinese medicinal materials (Chinese herbal medicine) have a long planting period, especially perennial root medicinal materials, and tissues rich in fat and wax, which are more susceptible to pollution by organochlorine pesticides. Although organochlorine pesticides have been banned in my country for many years, a large amo...

AI Technical Summary

Problems solved by technology

However, through nearly one year of detection practice, it has been found that although the pharmacopoeia method has high extraction efficiency, there are following deficiencies (1) due to the use of dichloromethane as the extraction agent, there is certain interference in the detection of organochlorine, although petroleum ether has been used many times The operation is removed, but the operation steps are increased, which increases the workload on the one hand, and introduces errors on the other hand

(2) After the purification step is sulfonated with concentrated sulfuric acid, the supernatant is directly taken for concentration, constant volume, and then enters the gas chromatograph for measurement. The residual concentrated sulfuric acid in the sample will greatly damage the capillary column and reduce the service life of the chromatographic column. ; At the same time, it will also cause certain pollution to the instrument inlet

(3) The process is complicated and the operation is cumbersome

However, the detection method of organochlorine residues in the national standard is not only cumbersome to operate, but the chromatographic column purification method is not suitable for samples containing a large amount of pigments, oils, and impurities such as Chinese herbal medicines. If the purification is not proper, many and large impurity peaks will greatly interfere with the detection. result

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