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Method for detecting trace N-nitrosamine in water

A detection method, a technology of nitrosamines, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve problems such as difficult detection, achieve the effect of simple steps, low price, and good promotion prospects

Inactive Publication Date: 2018-05-08
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Since N-nitrosamines have a high octanol / water partition coefficient and are often present in water in trace concentrations, it is difficult to detect them
At present, there is no unified method for detecting trace N-nitrosamines in water in my country, so it is extremely urgent to explore a detection method for trace N-nitrosamines in water with low detection limit, convenient operation, and low determination cost. of

Method used

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  • Method for detecting trace N-nitrosamine in water
  • Method for detecting trace N-nitrosamine in water
  • Method for detecting trace N-nitrosamine in water

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1) GC-MS test conditions

[0053] The standard solution (2.0 mg / L) of nine kinds of N-nitrosamines was analyzed by GC-MS, the ion source was EI source, the electron energy was -70eV, the carrier gas was high-purity helium, and 1 L of splitless injection was used. The temperature of the injection port in the experiment was 250°C, the temperature of the transfer line was 280°C, the temperature of the ion source was 210°C, and the flow rate of the carrier gas was 2.0 mL / min. GC / MS temperature programming conditions for N-nitrosamines: the initial column temperature is set to 35°C, kept for 4 minutes, raised to 220°C at a rate of 8°C / min, then raised to 280°C at a rate of 40°C / min, kept 2min. Using retention time and characteristic fragment ions to qualify, selected ion detection (SIM) and internal standard method to draw a standard curve for quantitative analysis, the GC-MS analysis parameters of different N-nitrosamines are as shown in Table 1, different N-nitrosamines ...

Embodiment 2

[0080] Determination of 9 kinds of nitrosamines in simulated water samples

[0081] Use 9 kinds of N-nitrosamine mixed standard (2000mg / L methanol solution) and NDMA-d of Supelco company 6 (1000mg / L dichloromethane) to prepare a mixed aqueous solution (total N-nitrosamine content 0.5μg / L, NDMA-d 6 Content 100ng / L) 1L, according to the method for embodiment 1 step 3-1)~3-5) water sample is processed, obtains the water sample to be tested, under the test condition of embodiment 1 step 1) to be tested water sample Perform detection, and calculate the content and recovery rate of each N-nitrosamine in the simulated water sample according to the detection result and the corresponding standard curve. Set up three parallel experiments, 9 kinds of nitrous and NDMA-d 6 The recovery experimental result is as shown in table 3:

[0082] Table 3 Nine kinds of nitrous and NDMA-d 6 recovery rate

[0083]

[0084]

[0085] It can be seen from Table 3 that except for the last NDphA,...

Embodiment 3

[0088] Determination of Simulated Precursor Nitrosamine Chloride

[0089] Nizatidine (stomach drug) is identified as one of the precursors of nitrosamines. Use deionized water to prepare 1 L of 24 μg / L nizatidine solution. At 25°C, under the condition of solution pH=8, 1L of nizatidine solution and 2mL of monochloramine solution with a concentration of 1.8g / L were chlorinated in the dark for 24h, then adding quencher, adding NDMA-d 6 As an internal standard (addition amount 100ng / L), it is pretreated according to the method of embodiment 1 step 3-1) ~ 3-5) to obtain the water sample to be tested, in the test condition of embodiment 1 step 1) Next, the water sample to be tested is detected, and the content of N-dimethylnitrosamine (NDMA) and NDMA-d in the water sample are calculated according to the detection result and the corresponding standard curve. 6 The recovery rate and the molar conversion rate of nizatidine, three groups of parallel experiments are set, and the resul...

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Abstract

The invention belongs to the field of environment detection and analysis and in particular relates to a method for detecting trace N-nitrosamine in water. The method comprises the following steps: a)mixing a water sample to be tested with N-nitroso-dimethylamine-d6, feeding through an activated carbon solid-phase extraction column, extruding off moisture in the activated carbon solid-phase extraction column, further eluting the activated carbon solid-phase extraction column with dichloromethane, and collecting an eluent; b) mixing the eluent with methanol, concentrating so as to obtain a concentrated liquid, mixing the concentrated liquid with N-nitroso-dimethylamine-d14 so as to obtain a sample to be analyzed; c) performing gas chromatography-mass chromatography detection on the sample to be analyzed, and calculating the type and the content of N-nitrosamine in a water sample to be detected according to detection results and standard curves established in advance. The method providedby the invention is simple and convenient in water sample pretreatment step, easy to operate, relatively low in price of GC-MS (Gas Chromatography-Mass Chromatography) equipment used in sample analysis, and relatively good in popularization prospect.

Description

technical field [0001] The invention belongs to the field of environmental detection and analysis, and in particular relates to a detection method of trace N-nitrosamines in water. Background technique [0002] N-nitrosamines are a class of compounds with potential carcinogenicity. Since precursor compounds such as nitrite and organic nitrogen undergo nitrosation or oxidation reactions in water to form N-nitrosamines, these compounds have a high detection rate in foreign tap water and pipe network end water, causing received widespread attention. [0003] Since N-nitrosamines have a high octanol / water partition coefficient and often exist in water in trace concentrations, it is difficult to detect them. At present, there is no unified method for detecting trace N-nitrosamines in water in my country, so it is extremely urgent to explore a detection method for trace N-nitrosamines in water with low detection limit, convenient operation, and low determination cost. of. Cont...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/08
CPCG01N30/02G01N30/06G01N30/08G01N30/72G01N2030/062
Inventor 金腊华王佳仪
Owner JINAN UNIVERSITY
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