Method for simultaneous determination of levo-glucan, mannan and galactan in aerosol by high performance liquid chromatography-tandem quadrupole mass spectrometry

A technology of high performance liquid chromatography and levodextran, which is applied in the directions of measuring devices, instruments, scientific instruments, etc., to achieve the effect of reducing use, saving scientific research costs, and good detection effect

Active Publication Date: 2018-10-23
何俊
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Problems solved by technology

The above detection limits are limited for the detection of aerosol samples in areas with less aerosol pollution or in weather with low aerosol concentration

Method used

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  • Method for simultaneous determination of levo-glucan, mannan and galactan in aerosol by high performance liquid chromatography-tandem quadrupole mass spectrometry
  • Method for simultaneous determination of levo-glucan, mannan and galactan in aerosol by high performance liquid chromatography-tandem quadrupole mass spectrometry
  • Method for simultaneous determination of levo-glucan, mannan and galactan in aerosol by high performance liquid chromatography-tandem quadrupole mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Precisely weigh 1.0 mg each of levoglucosan, galactan, and mannan, dissolve with an appropriate amount of ultrapure water, transfer to a 100ml volumetric flask, and dilute to the mark with ultrapure water. Shake well and let stand to obtain 10μg / ml L, M, G mixed standard solution. The solutions used for the test working curves of L, M, and G are diluted step by step from the above 10μg / ml standard solution, respectively prepared into a series of solutions of 0.005, 0.01, 0.02, 0.05, 0.1, 0.2, 0.5, 1μg / ml, and then press the above Experimental conditions: High performance liquid chromatography-tandem quadrupole mass spectrometer HPLC-MSMS analysis and detection, the mobile phase is selected as ammonia water and ultrapure water (10:90, v / v) with a mass fraction of 0.001%, and the constant flow rate is set to 0.4 ml min -1 , the temperature of the column oven was 45°C. The optimal ion spray voltage is set to -3800V, the atomizing gas is set to 38psi, the atomizing temper...

Embodiment 2

[0037] Cut the high-flow air particle sampling filter membrane 3cm×3cm, cut it into pieces, add 3ml ultrapure water, and perform ultrasonic extraction for 45 minutes. After the extract was filtered through a 0.45 μm hydrophobic PTFE needle filter, the filtered extract was tested and analyzed with a high performance liquid phase-tandem quadrupole mass spectrometer. The test analysis experiment condition is the same as embodiment 1, external standard method is quantitative. Three parallel samples were made to the air aerosol sample, the test numbers are A, B, and C, the analysis results are shown in Table 2, and the first parallel sample (test number A) was measured 5 times, and the analysis results are shown in Table 3. As can be seen from Table 2, the relative standard deviation (RSD) of L in the parallel sample is 8.98%, the relative standard deviation of M is 12.43%, and the relative standard deviation of G is 6.98%; The relative standard deviation is 1.31%, the relative st...

Embodiment 3

[0044] The standard solution in Example 1 was added to the prepared test solution with known negative results (the test did not contain the target compound), and the experiment was carried out according to the instrumental analysis and detection method in Example 1. This sample is done 10 parallel measurements to get the average value, according to the actual addition and the measured results, calculate the recovery rate of the sample, the test results are shown in Table 4, as can be seen from Table 4, the recovery of the standard addition of levoglucosan in the sample The rate reaches between 97-101%, and the relative standard deviation of parallel measurement is 0.95%; The spiked recovery of lactan was between 99-100%, and the relative standard deviation of parallel measurement was 0.47%;

[0045] Table 4 The recovery of standard addition of this sample

[0046]

[0047]

[0048] figure 1 It is the chromatogram of L, M and G detected in Example 1 of the present inven...

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Abstract

A method for synchronously measuring levoglucosan, mannan and galactosan in aerosol for high performance liquid chromatography-tandem quadrupole mass spectrometry combination includes the steps that levoglucosan, mannan and galactosan in an aerosol sample are subjected to ultrasonic extraction with ultrapure water and detected by means of a high performance liquid chromatography-tandem quadrupolemass spectrometer; ammonia water is adopted as a mobile phase; an electrospray ionization mode suitable for polar molecule analysis is adopted as an ion source of a mass spectrometry, ion source parameters and compound parameters optimized many times are adopted in a mass spectrometric method, and qualitative and quantitative analysis is conducted in an anion and multiple-reaction monitoring mode.By means of the external standard curve method, the linear relation of L, M and G is good in the range of 0.01<-1> microgramme per milliliter, the correlation coefficient is larger than 0.99, the detection limit of L is smaller than 0.005 microgramme per milliliter, the detection limits of M and G are both smaller than 0.01 microgramme per milliliter, experiment repeatability is good, relative standard deviations of repetitive experiments of L, M and G are 1.31%, 4.48% and 1.31% respectively, and the adding standard recovery rates of L, M and G all reach 97% or above.

Description

technical field [0001] The invention relates to a method for synchronous determination of levoglucosan, mannan and galactan in aerosol by high performance liquid chromatography-tandem quadrupole mass spectrometry. Background technique [0002] Biomass combustion, such as forest fires and straw burning, will emit toxic substances such as polycyclic aromatic hydrocarbons and halogenated organic pollutants, which will affect human health. At the same time, it will also emit greenhouse gases and atmospheric particles, which will affect the atmospheric environment and climate change. The composition is extremely complex, so it is very important to use molecular tracers to study the impact of material combustion on the atmospheric environment in regional or local areas. [0003] Levoglucosan (1,6-anhydro-β-d-glucose, or Levoglucosan, L) scientific name 1,6-anhydro-β-D-glucose, is a product of cellulose pyrolysis above 300 ° C, There is no other source. It is widely used as a tra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 何俊徐婧莎徐宏辉姜瑜君
Owner 何俊
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