Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of lc-ms analysis method of acid chloride derivatives

A LC-MS and derivative technology, applied in the field of medicine and chemical industry, can solve the problems of undetermined fragment ions, poor method reproducibility, and slow reaction of derivative reactions, etc.

Active Publication Date: 2022-07-08
SUNSHINE LAKE PHARM CO LTD
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Gas chromatography-mass spectrometry method: alcohols with small molecular weight such as methanol and ethanol are commonly used to esterify acid chlorides and then detect them. When the detection limit is very low, the derivatization reaction is slow at room temperature, and the conversion rate of acid chlorides is relatively low. Fragment ions cannot be determined, the interference factors are large, and the method reproducibility is poor
[0007] Liquid chromatography-mass spectrometry: For the alkyl acid chloride compounds whose detection limit requirement is <1.5, there is currently no suitable derivatization reagent so that the derivative product has a better response value in LC-MS

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of lc-ms analysis method of acid chloride derivatives
  • A kind of lc-ms analysis method of acid chloride derivatives
  • A kind of lc-ms analysis method of acid chloride derivatives

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach

[0067] In order for those skilled in the art to better understand the technical solutions of the present invention, some non-limiting examples are further disclosed below to further illustrate the present invention in detail.

[0068] The reagents used in the present invention can be purchased from the market or can be prepared by the method described in the present invention.

[0069] The analytical reagents and solutions used in the present invention meet the requirements of the appendix of the 2010 edition of the Chinese Pharmacopoeia, unless otherwise specified.

[0070] In the following examples, the test sample is the sample to be tested.

Embodiment 1

[0071] Embodiment 1 Verification of ethyl chloroformate residual method in ritonavir

[0072] Instruments, reagents, reference substances and test substances:

[0073] Instruments: 1 / 100,000 analytical balance, liquid chromatography-mass spectrometer;

[0074] Reagent: dichloromethane (HPLC grade);

[0075] Control substance: ethyl chloroformate (AR grade)

[0076] Derivative: N,N-diisopropylethylenediamine

[0077] Test article: ritonavir

[0078] Solution preparation:

[0079] Blank solution / diluent: take about 20mg of N,N-diisopropylethylenediamine into a 25ml volumetric flask and shake well; take an appropriate amount into a liquid phase vial;

[0080] Reference substance mother liquor 1: Take about 39.06 mg of ethyl chloroformate (limit of 1.25), accurately weigh it, put it into a 50 mL volumetric flask, dissolve it with dichloromethane and dilute to volume, shake well;

[0081] Reference substance mother solution 2: Precisely pipette 1.0 mL of reference substance m...

Embodiment 2

[0155] Embodiment 2 Determination of ethyl chloroformate residual content in azilsartan medoxomil

[0156] Instruments, reagents, reference substances and test substances

[0157] Instruments: 1 / 100,000 analytical balance, liquid chromatography-mass spectrometer;

[0158] Reagent: dichloromethane (HPLC);

[0159] Control: Ethyl Chloroformate (AR)

[0160] Derivative: N,N-diisopropylethylenediamine

[0161] Test article: Azilsartan

[0162] Solution preparation

[0163] (1) Blank solution / diluent: take about 20 mg of N,N-diisopropylethylenediamine, put it into a 25ml volumetric flask, add dichloromethane to the volume and shake well; take an appropriate amount and put it into a liquid phase vial;

[0164] (2) Reference substance mother liquor 1: Take about 37.5 mg of ethyl chloroformate, accurately weigh it, put it into a 10 mL volumetric flask, dissolve it with dichloromethane, and dilute to volume, shake well;

[0165] (3) Reference substance mother solution 2: Precisel...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a method for measuring acid chloride derivatives by LC-MS, using N,N-diisopropylethylenediamine as a derivatizing reagent to detect acid chloride derivatives, and the derivatization reaction is completed rapidly. The method is characterized in that a chromatographic column with octadecylsilane bonded phase is used as the stationary phase; the mobile phase is composed of phase A and phase B, wherein the mixture of buffer salt solution and organic solvent is used as phase A, and the organic solvent is used as phase A. As phase B, gradient elution was performed in a LC-MS system. The method provided by the invention has the advantages of high efficiency, convenience, good specificity and high sensitivity.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and more particularly relates to a method for measuring acid chloride compounds by LC-MS. Background technique [0002] Acid chloride refers to a compound containing -C(O)Cl functional group, which belongs to a class of acid halides. It is a carboxylic acid derivative formed after the hydroxyl group in the carboxylic acid is replaced by chlorine. The acid chloride is very unstable. [0003] Among the common detection methods, the titration method is only used for macrochemical analysis methods, and cannot meet the detection requirements for trace substances. [0004] Gas chromatography: Acyl chloride has strong reactivity, which is easy to cause damage to the packing of the chromatographic column, and direct injection will cause great damage to the chromatographic column; at the same time, the molecular weight of the alkyl acyl chloride is relatively large and the boiling point is re...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/067
Inventor 曹继陆秀丽巢燕芳游孟梦熊学武刘国柱
Owner SUNSHINE LAKE PHARM CO LTD