Determination of residual solvents in the drug famciclovir by gas chromatography

Abstract: Famciclovir (Famciclovir) is a diethyl acyl lipid of the 6-deoxy derivative of penciclovir (C14H19N5O4). It has good oral absorption and high bioavailability, so it replaces penciclovir.

The main features of GC-5890 gas chromatograph:

1. Fully compatible with HP HP5890II gas chromatograph, can be directly connected to HP5890 miniature monofilament thermal conductivity detector, hydrogen flame ionization detector and related detector control board. Instrument technical indicators, performance, detector sensitivity are comparable to HP5890 !

2. New integrated digital electronic circuit, high control accuracy, stable and reliable performance, and temperature control accuracy up to 0.01 ℃.

3. The unique sample inlet design solves the sample discrimination; the dual-column compensation function not only solves the program drift caused by heating, but also reduces the influence of background noise, and can get a lower minimum detection limit.

4. The volume of the oven is large, and the intelligent rear door opening system has stepless variable air intake and output, which shortens the system stable equilibrium time after the program rises / cools; , The heating rate is 0-50 ℃ / min; the increment of 0.1 ℃ / min can be recalibrated by the user, and the maximum temperature can be set at will. The user decides the temperature balance time of the heating furnace.

5. Two sampling systems can be installed at the same time: packed column, capillary split / splitless sampling system (with diaphragm cleaning function); two same or different detectors can be installed at the same time: hydrogen flame ionization detector (FID) , Thermal conductivity detector (TCD). Optional automatic / manual gas six-way sampling valve sampler, headspace sampler, thermal analysis sampler, methane conversion furnace.

Available testing instruments: GC headspace gas chromatograph, headspace sampler

Objective: To establish a content determination method for the residual solvents methanol, ethyl acetate, dichloromethane and n-hexane in the raw drug famciclovir. Method: Headspace gas chromatography, hydrogen flame ionization detector, water as solvent, butanone As an internal standard, the column is a quartz capillary column: HP-1 (30m × 0.32mm, film thickness 1.05μm).

Results: The four residual solvents have a good linear relationship (r = 0.9974 ~ 0.9999) in the concentration range corresponding to the limit of 50% to 150%, and the average recovery rate is 82.0% to 113.0%.

Conclusion: The method is simple, reliable and accurate, and can be used to control the residual solvent content of APIs.

Headspace sampling technology is a convenient and fast sample preparation method in gas chromatography. The principle is to place the sample to be tested in a closed container, and the volatile components are volatilized from the sample matrix by heating. Come out, reach equilibrium in the gas-liquid (or gas-solid) two phases, directly extract the top gas for chromatographic analysis, so as to check the composition and content of volatile components in the sample. The use of headspace sampling technology can eliminate the lengthy and cumbersome sample preparation process, avoid the interference of organic solvents on the analysis, and reduce the pollution of the chromatography column and the inlet. The DK300A headspace chromatography sampler developed by our company fills the gap of domestic instruments. This instrument can be connected to various types of gas chromatographs at home and abroad.

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