Method for performing parent ion scanning analysis by utilizing time multi-stage mass spectrometry

A parent ion scanning and parent ion technology, applied in the field of analysis and detection, can solve problems such as difficult to achieve parent ion scanning

Inactive Publication Date: 2013-09-25
BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the time multi-level mass spectrometry, there is only one space, and the ion capture, fragmentation and detection in the analysis process can only be completed in different time periods in t

Method used

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  • Method for performing parent ion scanning analysis by utilizing time multi-stage mass spectrometry
  • Method for performing parent ion scanning analysis by utilizing time multi-stage mass spectrometry
  • Method for performing parent ion scanning analysis by utilizing time multi-stage mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] In this embodiment, linear ion trap mass spectrometry is used to scan parent ions of sulfa drugs, and the specific steps are as follows:

[0039] a. Preparation of standard products:

[0040] As shown in Table 1, 16 kinds of sulfonamide standard substances were purchased from Dr. Ehrenstorfer Company, and the purity was more than 98%; the test water was Milli-Q ultrapure water, and other reagents were chromatographically pure; 16 kinds of sulfonamide standard substances Use 50% methanol aqueous solution to make a mixed standard solution of 100ng / mL.

[0041] b. Mass spectrometry conditions and parameter settings:

[0042] Mass analyzer: LTQ linear ion trap mass spectrometer; ionization method: ESI + ; Spray voltage: 4.5kV; Tubular lens voltage: 115V; Sheath gas (nitrogen) flow rate: 25arb; Auxiliary gas (nitrogen) flow rate: 3.00arb; Capillary temperature: 350℃; Precursor ion mass range (m / z): 200- 360, that is, the initial mass number is 200, and the end mass number...

Embodiment 2

[0061] In this example, linear ion trap mass spectrometry is used to scan precursor ions of the illegal drug sibutramine and its structurally similar drugs added to a weight loss health food on the market. The specific steps are as follows:

[0062] a. Sample description and pretreatment:

[0063] Take a commercially available slimming health food, capsules; the active ingredients marked in the package are: chitin, tea leaves, cassia seeds, lotus leaf, hawthorn, radices, betel nuts, green bark, vitamin C; scope of use: simple obesity, adolescent obesity , Postpartum obesity.

[0064] Take 0.1g of the drug powder in the capsule, add 10mL of 50% methanol aqueous solution, and mix well; 14000R, 5min high-speed centrifugation, take 10μL of the supernatant sample concentrated solution, use 50% methanol aqueous solution to dilute to a 10mL volumetric flask, and obtain the working solution of the sample , for precursor ion scanning analysis and LC-MS verification.

[0065] The test...

Embodiment 3

[0080] In this embodiment, linear ion trap mass spectrometry is used to scan the parent ion of the amino acid active agent in a commercially available cosmetic, and the specific steps are as follows:

[0081] a. Sample description and pretreatment:

[0082] Take a commercially available face-lifting functional cosmetic, liquid, take 10 μL sample concentrated solution, use 50% methanol aqueous solution to dilute to 10mL volumetric flask, and obtain the working solution of the sample, which is used for parent ion scanning and LC / MS analysis. The test water was Milli-Q ultrapure water, and other reagents were chromatographically pure.

[0083] b. Mass spectrometry conditions and parameter settings:

[0084] Precursor ion scanning conditions:

[0085] Mass analyzer: LTQ linear ion trap mass spectrometer; ionization method: ESI + ; Spray voltage: 4.5kV; Tubular lens voltage: 115V; Sheath gas (nitrogen) flow rate: 25arb; Auxiliary gas (nitrogen) flow rate: 3.00arb; Capillary temp...

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Abstract

The invention relates to a method for performing parent ion scanning analysis by utilizing time multi-stage mass spectrometry. The method comprises the following steps: (1) feeding samples by employing a syringe or a peristaltic pump, so that tested samples continuously enter a mass spectrum ion source; (2) selecting a daughter ion and a proper cracking energy; (3) setting an initial mass number, a final mass number and a stepping distance of parent ions in time multi-stage mass spectrometry; starting from the initial mass number, taking a certain mass number stepped each time as the stepping distance and stopping till the final number, continuously and selectively cracking parent ions entering a mass spectrometer, and recording information of the parent ions which can generate the daughter ion in the step (2); and (4) verifying the parent ions obtained in the step (3) by employing liquid chromatography tandem mass spectrometry. According to the method, parent ion scanning is realized in the time multi-stage mass spectrometry, so that the problem that the parent ion scanning is difficultly realized because only a detector exists in the time multi-stage mass spectrometry in the prior art is solved, and a false positive result is effectively eliminated.

Description

technical field [0001] The invention relates to a method for realizing parent ion scanning analysis by using time multi-level mass spectrometry, and belongs to the technical field of analysis and detection. Background technique [0002] Mass spectrometry is an important means to characterize and analyze unknown compound molecules. Among them, precursor ion scanning technology is a mass spectrometry method to find parent ion compounds containing the same product ion through a specific mass spectrometer program. Different from other research methods that use all product ions of the target parent ion as research objects, parent ion scanning technology focuses on It is used to find all precursor ion information with the same product ion, so that a series of compounds with the same structural characteristics can be effectively detected. Therefore, this method has important application value in new drug development, drug abuse detection, and in vivo metabolite analysis. . [000...

Claims

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Application Information

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IPC IPC(8): G01N27/62
Inventor 刘鑫张朝晖卢晓宇严华李建辉张海燕杨金良
Owner BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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