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A kind of determination method of residual solvent in calf serum deproteinized injection

A calf serum and determination method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of ethanol and methanol solvent analysis interference, shortened service life, column pollution, etc., to avoid interference of sample matrix and simple operation Feasible, avoid pollution effect

Active Publication Date: 2016-02-03
JINZHOU AHON PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since calf serum deproteinized injection contains non-volatile impurities such as metal ions and inorganic salts, the product directly enters the gas chromatography column, which will cause pollution to the column, reduce the separation effect of the column, and shorten the service life
Moreover, the product has complex components and may contain some volatile compounds similar to lipids, which may be decomposed at the gas chromatograph inlet. If some substances in these volatile compounds are detected by the detector, they may be harmful to ethanol and methanol. Solvent analysis causing interference

Method used

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  • A kind of determination method of residual solvent in calf serum deproteinized injection
  • A kind of determination method of residual solvent in calf serum deproteinized injection
  • A kind of determination method of residual solvent in calf serum deproteinized injection

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Embodiment 1, the impact of different polarity chromatographic columns on the peak shape of methanol and ethanol

[0051] Condition 1: Polar chromatographic column HP-INNOWAX (30.0m×0.53mm×1.0μm); the initial column temperature is 50°C, keep it for 2min, and then set the temperature at 1°C·min -1 The temperature was raised to 55°C and kept for 3 minutes; the temperature of the injection port was 200°C; the temperature of the detector (FID) was 250°C; the split injection was performed with a split ratio of 1:1; the carrier gas was nitrogen; the flow rate was 1.0ml·min -1; For headspace sampling, the equilibrium temperature of the headspace bottle is 80°C, the equilibrium time is 30min, the temperature of the transfer tube is 115°C, and the temperature of the injection loop is 105°C.

[0052] Condition 2: Medium polarity chromatographic column DB-624 (60.0m×0.32mm×1.80μm); column temperature is 50°C, keep for 2min, and then set at 1°C·min -1 The temperature was raised to...

Embodiment 2

[0055] Embodiment 2, the impact of different split ratios on the peak shape of methanol and ethanol

[0056] Fix all chromatographic conditions except split ratio: HP-INNOWAX capillary column (30.0m×0.53mm×1.0μm); -1 The temperature was raised to 55°C at a certain rate and kept for 3 minutes; the temperature of the injection port was 200°C; ℃, the injection loop temperature is 105℃; split injection, the split ratio is 1:1, 3:1, 5:1 or 10:1; the carrier gas is nitrogen, the flow rate is 1.0ml min -1 .

[0057] Other conditions were fixed, and the reference substance solution was analyzed with a split ratio of 1:1, 3:1, 5:1 or 10:1. The tailing factor is shown in Table 1:

[0058] Table 1 Split ratio and tailing factor

[0059] split ratio

[0060] It can be seen from Table 1 that with the increase of the split ratio, the peak shape is significantly improved. Under the condition of a split ratio of 5:1, the peak shape of the chromatographic peak is already very good...

Embodiment 3

[0061] Embodiment 3, the influence of headspace equilibrium temperature on methanol and ethanol peak area

[0062] Fix all chromatographic conditions except headspace equilibrium temperature: HP-INNOWAX capillary column (30.0m×0.53mm×1.0μm); -1 The temperature was raised to 55°C and kept for 3 minutes; the temperature of the injection port was 200°C; the temperature of the detector (FID) was 250°C; the split injection was performed with a split ratio of 5:1; the carrier gas was nitrogen; the flow rate was 1.0ml·min -1 . For headspace sampling, the equilibration time was 30 minutes, the temperature of the transfer tube was 115°C, and the temperature of the injection loop was 105°C. The chromatographic peak areas at the equilibrium temperature of the water in the headspace bottle were investigated at 65°C, 70°C, 75°C, 80°C, and 85°C. The results are shown in Table 2.

[0063] Table 2 Equilibrium temperature and peak area

[0064] Equilibrium temperature (℃)

[0065]...

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Abstract

The invention relates to a method for determining a residual solvent in a deproteinised calf serum injection. The method comprises the following steps: injecting a reference solution and a test solution into a chromatographic instrument in a headspace sampling manner; carrying out chromatography test by adopting a corresponding chromatography condition, and recording a chromatogram map; and carrying out qualitative and quantitative detection according to the chromatogram map. The sample measured by the method is free of special treatment, and pollution of a chromatographic column and interference of sample matrix can be avoided. The method is high in sensitivity, simple in operation, and suitable for detection of residual methanol and ethanol in an organic solvent in the deproteinised calf serum injection, reference is provided for controlling the residue of the organic solvent in the deproteinised calf serum injection production process, and the quality is ensured.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for determining residual organic solvents in calf serum deproteinized injections. Background technique [0002] Residual solvents in pharmaceuticals refer to organic solvents that cannot be completely removed during the production of raw materials or excipients, as well as during the preparation of preparations. In the 2010 edition of the Pharmacopoeia of the People's Republic of China, the second appendix VIIIP has certain requirements for the limits of organic solvents. However, at present, the country has only published guidelines for the residual solvents of chemical drugs, and has not issued guidelines for the determination methods and limit requirements of biochemical drugs. Therefore, it is of great significance to establish a detection method for solvent residues in biochemical drugs to control the quality of biochemical drugs. [0003] Calf serum deproteinized inje...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/16
Inventor 王鹏郭晶涛余江天马瑞国
Owner JINZHOU AHON PHARM CO LTD