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Method for quickly detecting picric acid in water by liquid chromatography-tandem mass spectrum

A tandem mass spectrometry and liquid chromatography technology, applied in the field of picric acid detection in water, can solve the problem of picric acid not being able to be effectively retained, and achieve the effects of less reagent dosage, good sensitivity and high recovery rate

Inactive Publication Date: 2012-01-04
宁波市环境监测中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a method for quickly detecting picric acid in water through liquid chromatography-tandem mass spectrometry, and to use a novel The affinity interaction column analyzes highly polar picric acid compounds, which solves the problem that picric acid cannot be effectively retained in reversed-phase liquid chromatography columns, and can achieve good retention of picric acid, and has high sensitivity and fast analysis speed , strong method selectivity, less pollution, simple operation, etc.

Method used

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  • Method for quickly detecting picric acid in water by liquid chromatography-tandem mass spectrum
  • Method for quickly detecting picric acid in water by liquid chromatography-tandem mass spectrum
  • Method for quickly detecting picric acid in water by liquid chromatography-tandem mass spectrum

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Experimental program
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Effect test

Embodiment 1

[0045] Standard curve drawing:

[0046] Use 9:1 acetonitrile / water solvent standard to prepare 1 μg / mL picric acid stock solution for later use. Then use 9:1 acetonitrile / water solvent to configure 0.1μg / L, 0.2μg / L, 0.5μg / L, 1μg / L, 2μg / L, 5μg / L and 10μg / L7 picric acid standard solutions for standardization Curve drawing. The result is as follows

[0047] Table 1 standard curve determination result

[0048]

Embodiment 2

[0050] Detection of picric acid in drinking water:

[0051] Take a drinking water sample and inhale about 0.9mL with a disposable sampling needle, dilute to 1mL with acetonitrile, filter through a 0.2μm organic phase needle filter, and directly inject it into a liquid phase sampling vial for testing. At the same time, take 10 μL of picric acid standard solution with a concentration of 0.1 mg / L, dilute to 1 mL with 9:1 acetonitrile and blank water sample, filter through a 0.2 μm organic phase syringe filter and set aside for use. The standard addition was repeated 7 times to obtain 7 spiked solutions to be tested.

[0052] The liquid to be tested was analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry, and the analysis conditions were as above. No picric acid was detected in the drinking water samples. The precision and recovery of the spiked samples are shown in the table below.

[0053] Table 2 Determination of precision and recovery of drinkin...

Embodiment 3

[0057] Detection of picric acid in wastewater:

[0058] The pretreatment is carried out by solid-phase extraction. The specific steps are: measure about 12mL of wastewater sample, adjust its pH value to 3.0 with acetic acid, filter through a 0.2μm filter membrane, and set the volume to 10mL. First use 5mL water and 5mL methanol to activate the solid-phase extraction column Waters Oasis HLB, 3mL, 60mg in sequence, and then pass 10mL of wastewater samples through the solid-phase extraction column at a speed of 3mL / min to enrich picric acid. , and continue vacuuming for 2 minutes to minimize the moisture remaining in the column. Finally, wash the extraction column with 9 mL of acetonitrile for 3 times to elute the picric acid, and dilute to 10 mL with water before entering the instrument for detection.

[0059] The liquid to be tested was analyzed by ultra-high performance liquid chromatography-tandem mass spectrometry, and the analysis conditions were as above. The content of ...

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Abstract

The invention discloses a method for quickly detecting picric acid in water by a liquid chromatography-tandem mass spectrum. The method comprises the following steps of: 1, pretreating the obtained water sample; and 2, analyzing and determining the treated water sample by an ultra performance liquid chromatography-tandem mass spectrum combined technology. The used liquid chromatography instrumentis an Acquity ultra performance liquid chromatography (UPLC) system and the picric acid is separated from the sample by the Acquity UPLC bridged ethylene hybrid (BEH) hydrophilic interaction liquid chromatography (HILIC) chromatographic column. The HILIC is used to keep the picric acid on the chromatographic column, and the picric acid is separated and detected in three minutes. The labeling experiment proves that the recovery rate of a drinking water sample reaches 94 to 105 percent and the recovery rate of a waste water sample reaches 79 to 97 percent in the method, and the requirement of picric acid determination in the water sample can be met. The method for quickly detecting picric acid in water by the liquid chromatography-tandem mass spectrum has the characteristics of high sensitivity, high analysis speed, strong selectivity, low pollution, and the like and is easy to operate.

Description

technical field [0001] The invention relates to a detection method for picric acid in water, in particular to a method for rapidly detecting picric acid in water through liquid chromatography-tandem mass spectrometry. Background technique [0002] In recent years, aromatic nitro compounds have been widely used in the fields of dyes, plastics, pesticides, pharmaceuticals and explosives. Studies have shown that it is toxic and carcinogenic, and has potential risks to humans and the environment. The microbial degradation process of aromatic nitro compounds in the environment often results in the conversion of nitro groups to amino groups, increasing toxicity and polarity, creating greater risks in the environment. In recent years, research on aromatic nitro compounds and their environmental metabolites has become a hot spot, especially on trinitrotoluene (TNT) and its metabolites, but for 2 , 4,6-trinitrophenol (2,4,6-trinitrophenol) research on analytical methodology is rela...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/08
Inventor 冯加永朱丽波钱飞中赵倩
Owner 宁波市环境监测中心
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