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Chinese herbal medicine residual organochlorine insecticide detection method
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A detection method, organochlorine technology, applied in the detection field, can solve problems such as cumbersome operation, detection interference, improper purification, etc.
Inactive Publication Date: 2008-08-13
JING BRAND
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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 petroleumether 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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Embodiment 1
[0066] Example 1 Detection of Residual Organochlorine Pesticides in Radix Astragali
[0067] One, the preparation of reference substance solution
[0068] Precisely absorb α-666, β-666, γ-666, δ-666, pentachloronitrobenzene, p, p, -DDT, p, p ,-DDD, p, p,-DDE, o, p,-DDT standard stock solution (petroleumether) 10ul in a 10ml volumetric flask, dilute to the mark with n-hexane, and mix well on a vortex shaker to obtain Concentration of 1ug / ml reference substance mixed solution, placed in the refrigerator for storage.
[0069] (2) Main experimental instruments, chromatographic conditions and reagents
[0097] The detection of the residual organochlorine pesticide in the Angelica medicinal material of embodiment 2
[0098] (1) The preparation of reference substance solution is the same as in Example 1
[0099] (2) Experimental apparatus, chromatographic conditions and reagents are the same as in Example 1
[0100] (3) the detection of reference substance solution is the same as in Example 1
[0101] (4) Preparation of the test product
[0102] Take Angelica sinensis (produced in Gansu, batch number 20060718) at a constant temperature of 60°C, grind it into fine powder, weigh 5g of the test samplepowder, weigh it accurately, add 30ml of acetone to a 100ml Erlenmeyer flask with a stopper, shake well, and soak overnight , ultrasonic extraction for 20min, twice, add 30ml of petroleum ether, shake well, ultrasonic for 20min, let stand to cool, filter into a 250ml separating funnel, plug the triangular flask with 10ml of petroleum ether, pour all the filter residue into the tria...
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Abstract
The present invention provides a method for examining residual organochlorine pesticides in Chinese traditionalmedicine, 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 petroleumether, 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...
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