Method for detecting levoglucosan in water sample by using ultra-high performance liquid chromatography-triple quadrupole mass spectrometer

An ultra-high performance liquid phase, triple quadrupole technology, applied in the field of levo-glucan content, can solve the problems of difficult and accurate detection, difficult to enrich, concentrate or extract, avoid pollution or loss, avoid mass spectrum peak broadening or Matrix effect, effect of stable response

Pending Publication Date: 2020-08-25
NORTHWEST UNIV
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Problems solved by technology

[0004] In aqueous samples such as ice and snow samples, the content of levoglucosan is often at the ppb level or even lower, and l

Method used

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  • Method for detecting levoglucosan in water sample by using ultra-high performance liquid chromatography-triple quadrupole mass spectrometer
  • Method for detecting levoglucosan in water sample by using ultra-high performance liquid chromatography-triple quadrupole mass spectrometer
  • Method for detecting levoglucosan in water sample by using ultra-high performance liquid chromatography-triple quadrupole mass spectrometer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Sample preparation

[0030] Using ultrapure water and standard products of levoglucosan, prepare levoglucosan with concentrations of 0.25ng / mL, 0.5ng / mL, 1ng / mL, 5ng / mL, 10ng / mL, 20ng / mL, and 50ng / mL, respectively standard solution in water.

[0031] The ice core sample to be tested is processed into a single sample in a 100-class ultra-clean workbench, and the outer layer of about 2cm icicles is removed with a special ultra-clean tool. Place in ethylene glycol formate (PET) bottle and let it melt at room temperature.

[0032] Clean the sampling vial with ultrapure water and methanol repeatedly ultrasonically, and dry it in a class 100 ultra-clean workbench, then use a pipette to take 300 μL of levoglucosan standard aqueous solution of different concentrations and the melted ice core to be tested Samples, respectively, were injected into the injection vials and capped to seal.

[0033] 2. Sample testing

[0034] Agilent 1290-6470 ultra-high performance liquid chr...

Embodiment 2

[0037] According to the method of embodiment 1, the snow water sample is detected, and the detection results are shown in Figure 5 , the levoglucosan concentration in the snow water sample was 20.3160ng / mL.

[0038] In order to prove the beneficial effect of the method, the inventors used levoglucosan standard aqueous solution and a plurality of samples of different concentration levels to carry out methodological verification, and the specific tests were as follows:

[0039] 1. Method reproducibility

[0040] The reproducibility of this method was evaluated by detecting the same sample at different times and calculating the variation range of the response intensity. , according to the method of Example 1, select 5ng / mL levoglucosan standard aqueous solution and concentration to be the sample of 7.024ng / mL to carry out method reproducibility test, the same concentration standard substance three determination results of different time preparation are calculated as The RSD va...

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Abstract

The invention discloses a method for detecting levoglucosan in a water sample by using an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer. According to the method, parent ions are used as quantitative ions, daughter ions are used as qualitative ions, and the method has good sensitivity and accuracy. Compared with an existing method, the method adopts an external standard method for quantification, pollution caused by the environment, sample treatment, utensils and the like in the detection process can be detected and eliminated in time, and the reliability of adetection result is greatly improved; meanwhile, the method does not perform complex treatment on the sample, so that the accuracy and the reliable recovery rate of sample detection are ensured; moreover, the sample size of the method is only 2 [mu] L, so that the method is very suitable for detecting limited samples. Through calculation, the detection limit of the method is about 0.05 ng/mL, andthe quantification limit is about 0.2 ng/mL.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis methods, and in particular relates to a method for detecting levoglucosan content in water samples by using an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer. Background technique [0002] Levoglucosan (Levoglucosan, LGA, C 6 h 10 o 5 , 1,6-anhydro-β-D-glucose) is one of the most abundant monosaccharide anhydrides (MAS) formed by the combustion of cellulose or hemicellulose above 300°C, because it can exist stably in the air for several Ten hours to several days, and the degree of degradation is very small under anoxic or anaerobic conditions, such as levoglucosan in ice cores or in sediments, so it is an ideal tracer in the study of biomass combustion products , can be used as a record carrier for paleoclimate research or biomass burning at different times. [0003] Levoglucosan widely exists in aerosols, surface water, groundwater, snow and ice...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/72
CPCG01N30/02G01N30/06G01N30/54G01N30/72G01N2030/047
Inventor 姚秀南王宁练
Owner NORTHWEST UNIV
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