High-performance liquid chromatography for detecting residual amount of matrine in tobacco

A high-performance liquid chromatography and detection method technology, which is applied in the field of high-performance liquid chromatography detection of matrine residues in tobacco, can solve the problems of unsatisfactory purification effect, deviation of results, poor effect of impurities, etc., and achieve good purification effect of impurities , good accuracy and less impurity peaks

Inactive Publication Date: 2013-06-19
TOBACCO RES INST CHIN AGRI SCI ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The detection practice found that although this method of residue analysis is simple to operate, it has the following shortcomings: 1) It is only suitable for simple matrices, and the effect of removing impurities in tobacco is poor, and it is not suitable for complex matrices containing a large amount of pigments, oils, and impurities; 2) ) has high requirements for instruments, and the detection cost is expensive, making it difficult to popularize and apply
The disadvantages of this method for detecting matrine residues in tobacco are: the amount of eluent used in the purification process is large, and many impurities in the tobacco leaves are eluted, resulting in unsatisfactory purification results. Impurity peaks can easily interfere with the detection results and affect Accuracy of test results
Due to the complexity of the tobacco sample itself, the existing methods for detecting matrine residues in drugs are difficult to meet the needs of the detection of matrine residues in tobacco, which can easily cause deviations in the results, affecting the final detection results and the accuracy of matrine residues in tobacco. Assessment of Fair Use of Tobacco

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  • High-performance liquid chromatography for detecting residual amount of matrine in tobacco
  • High-performance liquid chromatography for detecting residual amount of matrine in tobacco
  • High-performance liquid chromatography for detecting residual amount of matrine in tobacco

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: Detection of Matrine Residues in Fresh Tobacco Leaf

[0050] 1. Extraction

[0051] Weigh 10.0g of fresh tobacco leaf sample into a 250mL ground-mouth Erlenmeyer flask, add 60mL of dichloromethane, oscillate and extract for 1h, filter with filter paper, accurately measure 30mL of the filtrate and transfer it to a 100mL flat-bottomed flask, and place on a rotary evaporator for 45 Concentrate under reduced pressure to near dryness at ℃, dissolve the residue with 2 mL of dichloromethane, and wait for purification.

[0052] 2. Purification

[0053] The alumina SPE column (500mg / 3mL) was pre-rinsed with 5mL of dichloromethane, the sample concentrated solution was passed through the column at a speed of 1-2 drops / second, the concentrated bottle was washed with 6mL of dichloromethane and transferred to a solid-phase small column, discarded Remove the eluent, and finally elute with 12mL dichloromethane / methanol (9:1, V / V) eluent, collect the eluent in a 100mL flat-...

Embodiment 2

[0081] Example 2: Detection of Matrine Residues in Dried Tobacco Leaves

[0082] 1. Extraction

[0083] Weigh 4.0g of dry tobacco leaf sample into a 250mL ground-mouth Erlenmeyer flask, add 60mL of dichloromethane, oscillate and extract for 1h, filter with filter paper, accurately measure 30mL of the filtrate and transfer it to a 100mL flat-bottomed flask, and place on a rotary evaporator for 45 Concentrate under reduced pressure to near dryness at ℃, dissolve the residue with 2 mL of dichloromethane, and wait for purification.

[0084] 2. Purification

[0085] Alumina SPE column (500mg / 3mL) was pre-rinsed with 5mL dichloromethane, the sample concentrated solution was passed through the column at a speed of 1-2 drops / second, 6mL dichloromethane washed the concentrated bottle and transferred to a solid-phase small column, discarded Remove the eluent, and finally elute with 12mL dichloromethane / methanol (9:1, V / V) eluent, collect the eluate in a 100mL flat-bottomed flask, and ...

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Abstract

The invention provides a high-performance liquid chromatography for detecting the residual amount of matrine in tobacco. The high-performance liquid chromatography comprises the following steps that (1) preparing a standard matrine solution, including weighing a standard matrine of a certain mass, dissolving with methanol, titrating to obtain a standard stock matrine solution, and diluting the standard stock matrine solution stepwise to obtain standard work solutions with a series of concentration gradients; (2) extracting, including extracting the matrine in tobacco by using dichloromethane as an extracting agent; (3) purifying, including purifying an extract by using an alumina SPE (solid phase extraction) columella; (4) detecting by using the liquid chromatography; (5) establishing a standard curve; and (6) computing and analyzing the matrine residue. The high-performance liquid chromatography provided by the invention is characterized by being simple, accurate, rapid and reliable and is of great importance to controlling the residual amount of matrine in tobacco and guiding the safe and reasonable application of matrine to tobacoo.

Description

technical field [0001] The invention belongs to the technical field of trace analysis, and in particular relates to a high performance liquid chromatography detection method for matrine residues in tobacco. Background technique [0002] Matrine is a natural botanical pesticide extracted from the roots, plants, and fruits of the Chinese herbal plant Sophora flavescens through ethanol and other organic solvents. Matrine has contact killing and stomach poisoning effects. Once the pest touches it, it will paralyze the nerve center, and then make the protein of the insect body solidify, block the stomata of the insect body, and cause the pest to suffocate to death. Matrine has a wide spectrum of action, and has obvious control effects on armyworms, cabbage caterpillars, aphids, and red spiders on various crops. As an excellent botanical insecticide, matrine has played an important role in the control of crop pests in my country. However, with the extensive application of matrin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 李义强王秀国王凤龙孔凡玉孙惠青徐金丽徐光军郑晓
Owner TOBACCO RES INST CHIN AGRI SCI ACAD
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