Gas chromatography detection method of chloroethane in L-glutamic acid diethyl ester hydrochloride

A diethyl glutamate and detection method technology, applied in the field of medicine, to achieve reliable qualitative and quantitative analysis, good separation effect, and strong specificity

Active Publication Date: 2019-04-16
SHANDONG BOYUAN PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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  • Gas chromatography detection method of chloroethane in L-glutamic acid diethyl ester hydrochloride
  • Gas chromatography detection method of chloroethane in L-glutamic acid diethyl ester hydrochloride
  • Gas chromatography detection method of chloroethane in L-glutamic acid diethyl ester hydrochloride

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Experimental program
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Embodiment 1

[0030] 1 Instruments and materials

[0031] 1.1 Instrument: 7890A gas chromatograph (Agilent);

[0032] 2 Methods and results

[0033] 2.1 Chromatographic conditions

[0034] Chromatographic column: nitroterephthalic acid-modified polyethylene glycol column DB-FFAP (30m×0.32mm, 0.25μm), column temperature: programmed temperature rise, 23°C for 15min, rising at a rate of 10°C / min To 80°C, keep for 2min; carrier gas: nitrogen, flow rate: 1ml / min, mode: split flow, split ratio: 20:1, inlet temperature: 180°C.

[0035] Detector: electron capture detector (ECD), temperature 270°C.

[0036] The headspace conditions are: equilibrium temperature: 60°C, equilibrium time: 20min, quantitative loop temperature: 70°C, transfer line temperature: 80°C, headspace vial volume: 20ml, liquid volume: 5ml.

[0037] 2.2 Preparation of solution

[0038] 2.21 Preparation of reference solution

[0039] Accurately measure 1ml of ethyl chloride solution (0.1mg / ml methanol solution), put it in a 10...

Embodiment 2

[0065] Embodiment 2: the detection of actual sample

[0066] 1) Get the original drug of L-diethyl glutamate hydrochloride, dissolve it in water or make it to volume, and prepare a solution containing 0.1mg L-diethyl glutamate hydrochloride in 1ml, as the test solution;

[0067] 2) Take the methanol solution of ethyl chloride, dissolve it in water or make it to volume, and prepare 1 ml of ethyl chloride solution containing 0.1 μg / ml as the reference solution;

[0068] 3) get the need testing solution and reference substance solution that step 1) prepares, adopt the identical instrument and reagent with embodiment 1, according to the chromatographic condition shown in step 2.1, accurately measure need testing solution 5ml, put 20ml top Empty bottle, sealed, headspace sampling, gas chromatograph detection, record chromatogram;

[0069] 3) adopt external standard method, take peak area as index, calculate impurity ethyl chloride content in the L-glutamic acid diethyl ester hydro...

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Abstract

The invention discloses a gas chromatography detection method of chloroethane in L-glutamic acid diethyl ester hydrochloride. A L-glutamic acid diethyl ester hydrochloride sample is dissolved and thenheadspace sample injection is performed. A GC-ECD detection method is used to carry out qualitative and quantitative operation on the chloroethane in the L-glutamic acid diethyl ester hydrochloride and methodology validation is performed. The method has the advantages of high specificity, a rapid speed, sensitive performance and the like. In the invention, the method of carrying out qualitative and quantitative operation on the chloroethane in the L-glutamic acid diethyl ester hydrochloride through adopting the GC-ECD detection method is firstly established so that the quality of the L-glutamic acid diethyl ester hydrochloride can be conveniently controlled.

Description

technical field [0001] The invention relates to a gas chromatography detection method for ethyl chloride, an impurity in L-glutamic acid diethyl ester hydrochloride, which belongs to the technical field of medicine. Background technique [0002] L-diethyl glutamate hydrochloride is a key intermediate in the synthesis of pemetrexed disodium. Pemetrexed disodium is an antifolate preparation with a pyrropyrimidine core in its structure, which can inhibit the growth of tumors by destroying the normal metabolic process dependent on folic acid in cells and inhibiting cell replication. [0003] Ethyl chloride is the reaction material of L-diethyl glutamate hydrochloride, and ethyl chloride is a genotoxic impurity. http: / / toxnet.nlm.nih.gov / cpdb / clearly records half of ethyl chloride TD 50 It is 1810 (mg / kg / day), so the detection method of ethyl chloride in L-diethyl glutamate hydrochloride should be formulated to control the quality of L-diethyl glutamate hydrochloride. But aft...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 杜方鹏孙庆伟董占静王先菊闫玲玲刘旭晶
Owner SHANDONG BOYUAN PHARM CO LTD
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