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
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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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