Method for detecting 22 organochlorine pesticide residues in total glucosides of radix paeoniae alba by using gas chromatography-mass spectrometry technology

A gas chromatography and pesticide residue technology, applied in the field of detection of 22 kinds of organochlorine pesticide residues in total glucosides of paeony, can solve problems such as interference with pesticide residue detection, and achieve the effects of high accuracy, good linearity and accurate quantification.

Active Publication Date: 2020-09-25
NINGBO LIWAH PHARM CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main components of total glucosides of paeony are saponins, which are highly polar. If you refer to the conventional medicinal material pretreatment method to extract pesticide residues by soaking in acid water or acetonitrile and other polar solvents, the saponins will be simultaneously Extracted out, interfere with the detection of pesticide residues

Method used

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  • Method for detecting 22 organochlorine pesticide residues in total glucosides of radix paeoniae alba by using gas chromatography-mass spectrometry technology
  • Method for detecting 22 organochlorine pesticide residues in total glucosides of radix paeoniae alba by using gas chromatography-mass spectrometry technology
  • Method for detecting 22 organochlorine pesticide residues in total glucosides of radix paeoniae alba by using gas chromatography-mass spectrometry technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0093] Example 1: Examination of specificity

[0094] Preparation of 22 organochlorine pesticide residue stock solutions:

[0095] Weigh 10 mg of 22 reference substances, accurately weigh them, and place them in a 10 mL volumetric flask, dissolve them with acetone and make up to the mark, and prepare a 1 mg / mL stock solution; the pesticide residue standard stock solution is stored at -18°C;

[0096] Preparation of 1 μg / mL mixed reference solution: take 100 μL of the stock solution, dilute to 10 mL with acetone to obtain a 10 μg / mL mixed reference solution, take 1 mL and dilute it to 10 mL with acetone to obtain a 1 μg / mL mixed reference solution. See Schedule 1;

[0097] Preparation of 400ng / mL mixed reference solution: take 400 μL of the above 1 μg / mL mixed reference solution, add acetone to dissolve and dilute to 1 mL to obtain a 400ng / mL mixed reference solution;

[0098] Preparation of the test solution of total glucosides of paeony glucosides: direct sampling of total g...

Embodiment 2

[0108] Example 2: Investigation on the pretreatment of different fillers

[0109] Prepare ① 900 mg of anhydrous magnesium sulfate and 300 mg of silica gel into a 15 mL centrifuge tube with a stopper, ② 900 mg of anhydrous magnesium sulfate into another 10 mL centrifuge tube with a stopper, ③ a commercially available pesticide residue purification tube; add 6 mL of toluene, 1 ppm Residual mixed reference substance 100μL, vortexed for 1min, centrifuged at 4000r / min for 5min, took the supernatant, placed it on a nitrogen blower at 40°C water bath and nitrogen blown to dryness, added 1mL of toluene, vortexed and mixed evenly, and filtered with a 0.22μm microporous membrane. Filter and get the filtrate.

[0110] Chromatographic conditions: Column: HP-5MS (30m×0.25mm×0.25μm); programmed temperature: 60°C for 2min, 16°C / min to 150°C for 0min, 10°C / min to 200°C for 0min , 3 °C / min to 220 °C for 0 min, 25 °C / min to 290 °C for 8 min; injection port temperature: 250 °C; injection volume...

Embodiment 3

[0114] Example 3: Inlet temperature investigation

[0115] Preparation of 100ng / mL mixed reference substance solution: take 100 μL of the above 1 μg / mL mixed reference substance solution, add acetone to dissolve and dilute to 1mL to obtain 100ng / mL mixed reference substance solution;

[0116] Preparation of the standard solution of total glucosides of paeony glucoside: direct sampling of total glucosides of paeony, weigh 2 g of the test product, weigh it, put it in a 15 mL centrifuge tube with stopper, add 10 mL of toluene, and add 1 μg / mL mixed reference substance Solution 200μL, ultrasonic for 20min, centrifugation at 4000r / min for 5min, take the supernatant to a 15mL centrifuge tube, add 900mg anhydrous magnesium sulfate, 300mg silica gel, vortex for 1min, centrifuge at 4000r / min for 5min, take the supernatant, put it in 40 Blow nitrogen in a water bath until dry, add 2 mL of toluene to make the volume, pass through a 0.45 μm filter membrane, and get the filtrate;

[0117]...

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Abstract

The invention discloses a method for simultaneously detecting 22 organochlorine pesticide residues in total glucosides of radix paeoniae alba by using a gas chromatography-mass spectrometry technology. The method comprises the following steps: preparing a mixed standard solution, a test solution and a matrix standard curve solution; sequentially injecting the matrix standard curve solution and thetest solution according to chromatographic conditions and mass spectrometric conditions, and drawing a matrix standard curve of 22 organochlorine pesticide residues; and respectively substituting thepeak response intensity data of the test solution to respectively calculate and obtain the concentrations of 22 organochlorine pesticide residues in the test solution. According to the method, the linear fitting degree of 22 organochlorine pesticide residues in the range of 5-400 ng/mL is high, the recovery rate of the 22 organochlorine pesticide residues is 62%-128% when the concentration is 0.1mg/kg, the relative standard deviation is smaller than or equal to 15%, and the limit of quantification of the method is smaller than or equal to 0.05 mg/kg. The method is rapid, simple, convenient,high in sensitivity, high in precision, high in accuracy and suitable for analysis and detection of 22 organochlorine pesticide residues in the total glucosides of radix paeoniae alba.

Description

technical field [0001] The invention belongs to the field of chemical analysis and detection, in particular to a method for detecting 22 kinds of organochlorine pesticide residues in the crude drug of total glucosides of paeony by utilizing gas chromatography-mass spectrometry technology. Background technique [0002] Paeonia lactiflora is the dry root of Paeonia lactiflora Pall. of the Ranunculaceae plant. Excavated in summer and autumn, washed, removed the head, tail and fine roots, boiled in boiling water, removed the outer skin or peeled, then boiled, and dried in the sun. White peony has the functions of nourishing blood and regulating menstruation, astringing yin and relieving sweat, softening liver and relieving pain, and calming liver yang. For blood deficiency and chlorosis, irregular menstruation, spontaneous sweating, night sweats, hypochondral pain, abdominal pain, cramping pain in limbs, headache and dizziness. Paeonia lactiflora is susceptible to a variety of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 沈君子殷红傅鼎鼎武晓剑钱勇谢天培
Owner NINGBO LIWAH PHARM CO LTD
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