Two-dimensional array liquid phase chromatogram-mass spectrometry combination method

A liquid chromatography and two-dimensional array technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of separation time limitation and separation ability, and achieve the effect of simple structure, increased separation ability and wide application range

Inactive Publication Date: 2008-04-30
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

Short columns (Opiteck, G.J.; Jorgenson, J.W.; Anderegg, R.J. Anal. Chem. 1997, 69, 2283-2291; Opiteck, G.J.; Ramirez, S.M.; Jorgenson, J.W.; Moseley, M.A. Anal. Biochem. -361; Wagner, K.; Miliotis, T.; Marko-Varga, G.; Bischoff, R.; Unger, K.K. , T.; Morisaka, H.; Ikegami, T.; Hosoya, K.; Ishizuka, N.; Minakuchi, H.; Nakanishi, K.; Ueda, M.; Cabrera, K.; .2004, 27, 897-904), high-temperature HPLC (Stoll, D.R.; Carr, P.W.J.Am.Chem.Soc.2005, 127, 5034-5035) have been adopted successively, and it is undeniable that they have injected new elements into LC×LC , but the very short separation time limits their ability to separate
In order to fundamentally improve the separation ability of two-dimensional liquid chromatography, the analysis time of the second dimension should be appropriately increased, and the column length of the second dimension should be increased, but these are contrary to the traditional two-dimensional second-dimensional rapid separation concept , which is difficult to achieve by traditional comprehensive two-dimensional liquid chromatography

Method used

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  • Two-dimensional array liquid phase chromatogram-mass spectrometry combination method

Examples

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Effect test

Embodiment 1

[0020] Two-dimensional array liquid chromatography-mass spectrometry was used to analyze the chloroform extraction parts of the methanol extract of traditional Chinese medicine Yinchen.

[0021] In this experiment, CN column (250×4.6mm) was used for the first dimension, and C18 column (150×2.1mm) was used for the second dimension, and gradient elution of acetonitrile (B) and water-0.5% formic acid (A) was used for both dimensions. Due to the limited laboratory hardware, the offline "1+4" mode 2D-Array-HPLC / MS is currently used. That is, one cyano column is used in the first dimension, and four C18 columns are used in the second dimension. The chromatographic condition of the first dimension is that 15% B increases linearly to 75% B within 72 minutes, the flow rate is 1 mL / min, and the detection wavelength is 254 nm. The chromatographic condition of the second dimension is that 15% B rises linearly to 39% B within 20min, then linearly rises to 60%B within 30min, and finally ri...

Embodiment 2

[0026] Two-dimensional array liquid chromatography-mass spectrometry was used to analyze the n-butanol extraction parts of the methanol extract of traditional Chinese medicine Yinchen.

[0027]The same chromatographic system as that used in Example 1 was used to analyze the n-butanol part of the traditional Chinese medicine Capillary chinensis. The chromatographic condition of the first dimension cyano column is that 10% B rises linearly to 18% B in 16 minutes, then rises linearly to 45% B in 5 minutes, and then rises linearly to 100% B in 4 minutes, and the flow rate is 1mL / min , the detection wavelength is 254nm. The chromatographic conditions of the second dimension C18 column are 10% B linearly increased to 25% B within 18min, then linearly increased to 32%B within 14min, and then linearly increased to 65%B within 33min, the flow rate was 0.2mL / min , using full-wavelength scanning, the monitoring wavelength is 254nm. The mass spectrometry conditions of the second dimensi...

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Abstract

The invention relates to a high-efficiency high-flux method of connecting two-dimension array liquid chromatogram and mass spectrum. After separated by the first-dimension chromatogram, the analyzed sample enters the second dimension for further high-efficiency separation; the first dimension enters the second-dimension chromatogram from the flow interface through a single chromatographic column; the mobile phase of the second dimension is hit by a chromatogram pump and then is divided by a dividing device through the interface and then hit into the second-dimension chromatographic column. The second-dimension chromatographic column adopts the array mode, and each chromatographic column in the array is synchronously separated with the same chromatographic conditions, the outlet of each chromatographic column of the second dimension is connected with one channel of the multi-channel detector to conduct synchronous high-sensitivity detection. The invention has the advantages of large system peak capacity, high separating efficiency, sensitive detection, simple online classification, large commercial prospect and extensive analyzing object.

Description

technical field [0001] The invention relates to a multidimensional liquid chromatography analysis technique for complex samples, in particular to a two-dimensional array liquid chromatography-mass spectrometry method. Background technique [0002] With the deepening of research in recent years, people have realized that many trace components that are difficult to detect in complex samples may play an important role, so the total component analysis of complex samples (such as biological samples, environmental samples, natural herbal medicines, etc.) The hotspots and difficulties in the field of analytical chemistry are discussed. Multidimensional chromatography is recognized for its powerful separation capabilities. As one of the more mature technologies, comprehensive two-dimensional gas chromatography provides a strong technical support for the analysis of all components of volatile complex samples (Tranchida, P.Q.; Dugo, P.; Dugo, G.; Mondello, L.J.Chromatogr., A 2004 , ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/78
Inventor 梁鑫淼刘艳明徐青薛兴亚章飞芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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