Method for detecting pesticide residues in anti-inflammatory and analgesic bolus

A detection method and pesticide residue technology, applied to the detection field of 9 kinds of organochlorine pesticide residues in Pien Tze Huang

Active Publication Date: 2013-03-27
ZHANGZHOU PIEN TZE HUANG PHARM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no relevant research report on the residues of organochlorine pesticides in Pien Tze Huang

Method used

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  • Method for detecting pesticide residues in anti-inflammatory and analgesic bolus
  • Method for detecting pesticide residues in anti-inflammatory and analgesic bolus
  • Method for detecting pesticide residues in anti-inflammatory and analgesic bolus

Examples

Experimental program
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Effect test

experiment example 1

[0038] Experimental Example 1: Methodological Research

[0039] Taking the mixed reference solution and Pien Tze Huang 1007030 as samples, the influence of blank solvent, linearity, stability, precision, repeatability, accuracy and recovery were investigated respectively.

[0040] 1. Solvent blank test

[0041] Petroleum ether with a boiling range of 60-90°C as the extraction solvent was used as a blank sample to directly enter the gas chromatography to investigate the interference of petroleum ether solvent with a boiling range of 60-90°C. see attached results Figure 1~3 . attached figure 1 It is the chromatogram of petroleum ether with a boiling range of 60~90℃, attached figure 2 For the reference substance solution chromatogram, attached image 3 For the test solution chromatogram. It can be seen from the comparison of the figures that the blank solvent petroleum ether has no interference on the spectrum area of ​​the test solution.

[0042] 2. Linear inspection

...

Embodiment 1

[0085] 1. Gas chromatograph: Agilent 7890A, ultrasonic extractor: KQ-300E (300W, 40KHZ); rotary evaporator: Shenke R series; centrifuge: Jiangsu Water Town Model: 800, speed: 50C / S; Meite Le electronic analytical balance (XP205);

[0086] 2. Gas chromatography conditions: AB-1701 elastic quartz capillary column (30m×0.32mm×0.25um), 63 Ni-ECD electron capture detector; inlet temperature 230°C, detector temperature 300°C, injection volume 1ul, splitless; temperature program: initial temperature 80°C, 6°C per minute to 200°C, 4°C per minute Rise to 250°C and keep for 40 minutes; the number of theoretical plates calculated based on the α-BHC peak should not be less than 1×10 6 , the resolution of two adjacent chromatographic peaks should be greater than 1.5;

[0087] 3. Determination

[0088] A. Preparation of reference substance stock solution: weigh BHC (α-BHC, β-BHC, γ-BHC, δ-BHC), DDT (PP'-DDE, PP'-DDD, OP'-DDT, PP '-DDT) and pentachloronitrobenzene (PCNB) pesticide refere...

Embodiment 2

[0094] 1. Gas Chromatograph: Agilent 7890A, Ultrasonic Extractor: KQ-300E (300W, 40KHZ); Rotary Evaporator: Shenke R Series; Centrifuge: Jiangsu Shuixiang Model: 800, Speed: 50C / S; Mette Le electronic analytical balance (XP205);

[0095] 2. Gas chromatography conditions: AB-1701 elastic quartz capillary column (30m×0.32mm×0.25um), 63 Ni-ECD electron capture detector; inlet temperature 230°C, detector temperature 300°C, injection volume 1ul, splitless; temperature programmed: initial temperature 80°C, 6°C per minute to 200°C, 4°C per minute Raised to 250°C and held for 40 minutes; the number of theoretical plates should not be less than 1×10 calculated based on the α-BHC peak 6 , the resolution of two adjacent chromatographic peaks should be greater than 1.5;

[0096] 3. Determination

[0097] A. Preparation of reference stock solution: Weigh hexahexahexanol (α-BHC, β-BHC, γ-BHC, δ-BHC), DDT (PP'-DDE, PP'-DDD, OP'-DDT, PP' '-DDT) and pentachloronitrobenzene (PCNB) pesticide...

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Abstract

The invention provides a method for detecting pesticide residues in a traditional Chinese medicine, and particularly relates to a method for detecting 9 organic chloride pesticide residues in anti-inflammatory and analgesic bolus. According to the method provided by the invention, a gas chromatographic method is adopted for measurement through optimization and methodology study on a preparation method of samples to be tested and gas chromatographic measurement conditions. The method has higher precision and repeatability, good sensitivity and a large linear range, can meet the requirements on a sampling recovery test, obtains accurate and reliable measurement results, and can meet the requirements on detection of the organic chloride pesticide residues in the anti-inflammatory and analgesic bolus.

Description

technical field [0001] The invention relates to a method for detecting pesticide residues in traditional Chinese medicine, in particular to a method for detecting nine kinds of organochlorine pesticide residues in Pien Tze Huang. Background technique [0002] Drug safety issues are directly related to people's life safety, health and social stability. In order to reduce the amount of pesticide residues in Chinese medicinal materials and improve the competitiveness of Chinese traditional medicine products in the international market, the detection and analysis of pesticide residues is a very important part. Pien Tze Huang is a commonly used traditional Chinese medicine in my country. In order to effectively control the quality of Pien Tze Huang and ensure the drug safety of Pien Tze Huang, it is necessary to detect and analyze its pesticide residues. At present, there is no relevant research report on organochlorine pesticide residues in Pien Tze Huang. SUMMARY OF THE INVEN...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 潘杰黄进明于娟吴丽璇
Owner ZHANGZHOU PIEN TZE HUANG PHARM
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