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Steroid substance derivation method and its analysis detection method

A detection method, sterol-based technology, applied in the field of analytical chemistry, can solve problems such as poor detection sensitivity and many side reactions, and achieve high sensitivity, convenient operation, and good derivation effect

Inactive Publication Date: 2012-10-17
BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to overcome the defects of many side reactions and poor detection sensitivity of existing derivatization methods, the purpose of the present invention is to provide a derivatization method for sterols

Method used

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  • Steroid substance derivation method and its analysis detection method
  • Steroid substance derivation method and its analysis detection method
  • Steroid substance derivation method and its analysis detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Determination of Derivation Method

[0037] (1) Preparation of reagents

[0038] 2,6-Di-tert-butyl-4-methylphenol (BHT) methanol solution: Weigh BHT powder, dissolve it in methanol, and prepare 100ng / mL BHT methanol solution, which plays an antioxidant role during the detection process.

[0039] Sterol standard substance solution: Weigh 1.5-2.0 mg of 24-dehydrocholesterol, 7-encholestanol, stigmasterol, and cholestanol standard substance respectively, dissolve them in a small amount of n-hexane, and the resulting solution Mix well, continue to add n-hexane, and prepare a series of sterol standard solutions with concentrations (between 0.001-1.400mg / dL). The normal content of non-cholesterol steroid substances in human serum is between 0.02-1.00mg / dL. The concentration selected in the technical solution of the invention covers this concentration range.

[0040] 5α-cholestane n-hexane internal standard solution: Weigh 5α-cholestane powder and dissolve it in n-hexane to ...

Embodiment 2

[0057] Derivatization reagent

[0058] Select the derivatization reagent HMDS+TMCS+pyridine (3+1+9) and B STFA+TMCS (99+1) (volume ratio) commonly used in the derivatization of sterol substance hydroxyl group in conventional technology

[0059] Through common technical analysis, it is concluded that there is a significant difference between the derivatization effect (peak area of ​​characteristic peak) of HMDS+TMCS+pyridine derivatization reagent and BSTFA+TMCS derivatization reagent (tfigure 2 );From figure 2 It can also be seen from Table 2 that after MSTFA derivation, the coefficient of variation of the response factor (RRF) of the quantifier ion is small (within 10%), indicating that the derivation method has good repeatability.

[0060] Table 2 The relative influence factor (RRF) of three kinds of derivatization reagents

[0061]

Embodiment 3

[0063] Derivation temperature

[0064] The peak area ratio ( RRF) was used as the research object to investigate the variation of RRF with derivatization temperature.

[0065] The experiment was designed to derivate at room temperature (25°C), 40°C, 60°C, 80°C, 100°C, 120°C and other temperature points, and the derivation time was uniformly adopted for 1 hour. The results are as follows image 3 shown. Above 60°C, the response factor of the quantitative ion basically does not change, so 60°C is selected as the temperature of the derivatization reaction.

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Abstract

The invention relates to a steroid substance derivation method, the derivation method employs N-methyl-N-trimethylsilyl trifluoroacetamide (MSTFA) as a derivative reagent, the N-methyl-N-trimethylsilyl trifluoroacetamide is derived for 20-60 minutes under the temperature of 30-80 DEG C. The invention also relates to an application of the derivation method in a steroid substance qualitative and quantitative analysis. The invention also relates to an analysis detection method of the steroid substance, the above mentioned method can be employed for performing a derivation treatment on a sample to be measured. According to the invention, the MSTFA is taken as the derivative reagent, and the derived steroid substance possesses good repeatability and high sensitivity in a GC or GC-MS detection. In addition, the MSTFA is taken as the derivative reagent, no macroscopic sediment is generated, a single derivative reagent is used, and the operation is convenient.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a derivation method of sterol substances in a chemical analysis process and a qualitative and quantitative detection method thereof. Background technique [0002] In addition to cholesterol, human serum also contains a small amount of squalene and non-cholesterol steroids. Non-cholesterol steroids include precursors for cholesterol synthesis, such as: 24-dehydrocholestanol (Desmosterol), 7-encholesterol Lathosterol, and dietary phytosterols such as Campesterol, Stigmasterol, β-sitosterol and Cholestanol. The molecular structure of some sterols is as follows: [0003] [0004] 24-Dehydrocholesterol 7-encholestanol [0005] [0006] stigmasterol cholestanol [0007] Recent studies have found that squalene and cholesterol precursor sterols in serum can be used as cholesterol synthesis markers to reflect the body's endogenous cholesterol synthesis efficiency, and plant st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18G01N30/02G01N30/72
Inventor 王启辉刘洋张经华陈瞾刘奕忍郑春巍勾新磊周晓萍徐康
Owner BEIJING CENT FOR PHYSICAL & CHEM ANALYSIS
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