Method for detecting 153 pesticide residues in heart benefiting and pulse restoring particle

Abstract

The invention relates to a method for detecting 153 pesticide residues in a heart benefiting and pulse restoring particle. The method is a liquid chromatography-mass spectrometry method. The method comprises the following steps: preparing a sample solution, preparing a matrix mixed reference substance working solution, and detecting the solutions through using the high performance liquid chromatography-mass spectrometry, wherein the sample solution is prepared through the following steps: crushing the heart benefiting and pulse restoring particle, weighing 1.8-2.2 g of the heart benefiting and pulse restoring particle, adding 80-120 [mu]L of an internal standard solution with the concentration of 5 [mu]g / mL, adding 8-12 mL of water, infiltrating the particle for 28-32 min, adding 8-12 mL of an acetonitrile solution containing 0.08-0.12% of acetic acid, oscillating the obtained solution in a swirl mixing oscillator at a rate of 4000-6000 r / min for 1.8-2.2 min, adding 3-5 g of anhydrous magnesium sulfate and 0.08-1.2 g of sodium acetate, carrying out swirl shaking for 4-6 min, centrifuging the obtained solution at a speed of 4000-6000 r / min for 4-6 min, taking 0.8-1.2 mL of the obtained supernatant, adding the supernatant to a centrifuging tube which is filled with 140-460 mg of anhydrous sodium sulfate, 23-27 mg of PSA, 48-52 mg of C18 and 2.3-2.7 mg of GCB in advance, carrying out swirl shaking for 2-4 min, centrifuging the obtained solution at a rate of 4000-6000 r / min for 4-6 min, taking the obtained supernatant, and filtering the supernatant by a 0.2-0.24 [mu]m filter membrane.

Description

Technical field [0001] The invention relates to a method for detecting pesticide residues in traditional Chinese medicine preparations, and in particular to a method for detecting 153 kinds of pesticide residues in Yixinfumai granules. Background technique [0002] The primary quality characteristic of a drug is safety. In addition to the influence of its own material basis, the safety of traditional Chinese medicine is caused by the introduction of foreign harmful substances during growth, processing, storage, production and other links, and residual pesticides are one of them. The so-called pesticide residues: refers to the pesticide parent and special derivatives with toxicological significance that remain in the medicinal parts after being affected by the growth environment or using pesticides during the cultivation, processing, and storage of traditional Chinese medicines, such as degradation or transformation products and metabolites. and industrial impurities, etc. ...

AI Technical Summary

Problems solved by technology

[0018] QuEChERS is considered to be a multi-species, multi-residue detection method for residue analysis in high water content (80-95%) matrices. Due to the variety of chemical properties of samples that conflict with the properties of pesticide residues, food and environmental samples The multi-residue analysis of pesticides is prone to some separation problems. Moreover, there may be a large amount of chlorophyll, lipids, steroids and other compounds in the complex sample matrix, which will seriously interfere with the analysis of the sample.

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