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A kind of gas chromatographic detection method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride

A technology of diethyl glutamate and a detection method, which is applied in the field of medicine and achieves a highly specific effect

Active Publication Date: 2021-04-09
SHANDONG BOYUAN PHARM CO LTD
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But after retrieval, there is no report about the content gas chromatography detection method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride

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  • A kind of gas chromatographic detection method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride
  • A kind of gas chromatographic detection method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride
  • A kind of gas chromatographic detection method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride

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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 for ethyl chloride in L-glutamic acid diethyl ester hydrochloride. It dissolves the L-glutamic acid diethyl ester hydrochloride sample and then injects the headspace sample, and adopts the GC-ECD detection method to qualitatively and quantitatively analyze the ethyl chloride in the L-glutamic acid diethyl ester hydrochloride. The method has been validated, and the method has the advantages of strong specificity, rapidity and sensitivity. The present invention first establishes the qualitative and quantitative method of ethyl chloride in L-glutamic acid diethyl ester hydrochloride using GC-ECD detection method, which is convenient to control the quality of L-glutamic acid diethyl ester hydrochloride .

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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Patent Type & Authority Patents(China)
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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