Method for quickly screening pesticides, drugs and converting products in waste water at same time

A technology for transformation products and pesticides, applied in the field of analytical chemistry, can solve the problems of complicated operation, single, inapplicable, etc., and achieve the effect of short analysis time, high accuracy and comprehensive screening.

Active Publication Date: 2018-04-06
NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] China Patent No. 201410028583.9, the application for which the date of authorization announcement is 2016.08.10 has announced a method for detecting enrofloxacin metabolites in sea cucumbers. The method includes sample extraction, purification, drawing of a standard curve, instrument conditions and Structural analysis of metabolites, which uses liquid chromatography-tandem mass spectrometry-ion trap technology to accurately determine the predicted metabolites using the pMRM method, using QTrap's unique MRM-IDA-EPI working mode, the MRM diagram of the corresponding metabolites can be obtained , and get its MS 2 Mass spectrogram; ten kinds of metabolites including ciprofloxacin can be identified, but the workflow of using the MRM-IDA-EPI mode in the method of this application is: respectively measure the sample solution to be tested and the blank

Method used

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  • Method for quickly screening pesticides, drugs and converting products in waste water at same time
  • Method for quickly screening pesticides, drugs and converting products in waste water at same time
  • Method for quickly screening pesticides, drugs and converting products in waste water at same time

Examples

Experimental program
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Effect test

Embodiment 1

[0056] The method of quickly screening pesticides, medicines and their transformation products in waste water simultaneously of the present embodiment is as follows:

[0057] (A), firstly collect 1L of wastewater in and out of industrial sewage treatment plants, and use high performance liquid chromatography-time-of-flight mass spectrometry for analysis and detection. The analysis and detection steps are:

[0058] Membrane filtration: Pass the above wastewater through a glass vacuum filter, filter through a 1μm glass fiber filter membrane and a 0.45μm nylon filter membrane, this method can remove impurities above 0.45μm more quickly;

[0059] Solid-phase small column extraction: Oasis HLB small column is used to enrich pesticides, drugs and their transformation products in wastewater. Before enrichment, Oasis HLB small column needs to be activated with 10mL methanol and 10mL water. The flow rate of water samples during the enrichment process is controlled at 3-5mL / min, keep th...

Embodiment 2

[0109] The wastewater in this example comes from a domestic sewage treatment plant, and the operation steps of the method for rapid screening of pesticides, drugs and their transformation products in wastewater by high performance liquid chromatography-time-of-flight mass spectrometry are basically the same as in Example 1.

[0110] According to the screening, a total of 17 kinds of pesticides and drugs were identified, and the compounds were confirmed by purchasing standard samples according to the retention time and fragments of the compounds. The pesticides and drugs screened in Example 2 are shown in Table 5.

[0111] Pesticides and drugs screened out in Table 5 Example 2

[0112]

[0113] And to roxithromycin, lidocaine etc. adopt the method for targeted screening conversion product to identify 3 kinds of conversion products, adopt the method for non-target screening conversion product to identify 5 kinds of conversion products, the conversion in embodiment 2 Product i...

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Abstract

The invention discloses a method of quickly screening pesticides, drugs and converting products in waste water at the same time, belonging to the field of analytical chemistry. The method comprises the following steps: (a) carrying out analytic detection, namely analytically detecting a sample; (b) carrying out pesticide and drug identification, namely screening by adopting pesticide and drug database software to identify whether pesticides and drugs exist or not; and (c) carrying out identifying-non-targeted screening of the converting products, namely predicting the converting products of identified pesticides and drugs in the step (b) through software, carrying out secondary spectrogram analysis and compound screening on an index compound of pesticides and drugs to predict diagnostic ions, and analyzing and identifying the converting products by extracting corresponding chromatographic peaks on the compound comprising the diagnostic ions. According to the method, pesticides, drugs and converting products in waste water can be screened at the same time, and the screening speed is high, the range is wide and the accuracy is high.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and uses liquid chromatography-time-of-flight mass spectrometry technology to carry out a high-throughput identification and identification method for pesticides, drugs and their transformation products in wastewater. Background technique [0002] With the development of the economy, more and more pesticides and drugs are produced. These chemicals are widely used in daily life after production. Due to the strong polarity of pesticides and pharmaceutical compounds, they are easy to migrate through water bodies and enter natural water bodies. Therefore, the detection of pesticides and drugs in wastewater has always been the focus of research by personnel in this field. [0003] At present, domestic analysis and research on pesticide and drug compounds in wastewater is usually the direct standard sample quantification of the compound; because the standard sample is expensive, there are many types...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/8809
Inventor 韦斯王学兵于南洋郭惠卫徐伟张效伟于红霞
Owner NANJING UNIV
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