(Ph. Eur. method 2.4.24)
envy是什么意思The test procedures described in this general method may be ud:马会游泳吗
i. for the identification of the majority of Class 1 and Class 2 residual solvents in an active substance, excipient or medicinal product when the residual solvents are unknown;
ii. as a limit test for Class 1 and Class 2 solvents when prent in an active substance, excipient or medicinal product;
秦王怫然怒iii. for the quantification of Class 2 solvents when the limits are greater than 1000 ppm (0.1 per cent) or for the quantification of Class 3 solvents when required.
Class 1, Class 2 and Class 3 residual solvents are listed in general chapter 5.4. Residual solvents.
Three diluents are described for sample preparation and the conditions to be applied for head-space injection of the gaous sample onto the chromatographic system. Two chromatographic systems are prescribed but System A is preferred whilst System B is employed normally for confirmation of identity. The choice of sample preparation procedure depends on the solubility of the substance to be examined and in certain cas the residual solvents to be controlled.
The following residual solvents are not readily detected by the head-space injection conditions described: formamide, 2-ethoxyethanol, 2-methoxyethanol, ethylene glycol,
N-methylpyrrolidone and sulfolane. Other appropriate procedures should be employed for the control of the residual solvents.
When the test procedure is applied quantitatively to control residual solvents in a substance, then it must be validated.
Procedure
Examine by gas chromatography with static head-space injection (2.2.28).
Sample preparation 1 This is intended for the control of residual solvents in
water-soluble substances.
Sample solution (1) Dissolve 0.200 g of the substance to be examined in water R and dilute to 20.0 ml with the same solvent.
计算机实习报告Sample preparation 2 This is intended for the control of residual solvents in
water-insoluble substances.
Sample solution (2) Dissolve 0.200 g of the substance to be examined in网络桥接
N,N-dimethylformamide R (DMF) and dilute to 20.0 ml with the same solvent.北京汽车音响改装
Sample preparation 3 This is intended for the control of N,N-dimethylacetamide and/or N,N-dimethylformamide, when it is known or suspected that one or both of the substances are prent in the substance to be examined.
Sample solution (3) Dissolve 0.200 g of the substance to be examined in
1,3-dimethyl-2-imidazolidinone R (DMI) and dilute to 20.0 ml with the same solvent.
In some cas none of the above sample preparation procedures are appropriate, in which ca the diluent to be ud for the preparation of the sample solution and the static
工程概况怎么写head-space conditions to be employed must be demonstrated to be suitable.
Solvent solution (a) To 1.0 ml of Class 1 residual solvent solution CRS, add 9 ml of dimethyl sulphoxi
de R and dilute to 100.0 ml with water R. Dilute 1.0 ml of this solution to 100 ml with water R. Dilute 1.0 ml of this solution to 10.0 ml with water R.
The reference solutions correspond to the following limits:
—benzene: 2 ppm,
—carbon tetrachloride: 4 ppm,
—1,2-dichloroethane: 5 ppm,
—1,1-dichloroethene: 8 ppm,
地狱神
—1,1,1-trichloroethane: 10 ppm.
Solvent solution (b) Dissolve appropriate quantities of the Class 2 residual solvents in dimethyl sulphoxide R and dilute to 100.0 ml with water R. Dilute to give a concentration of 1/20 of the limits stated in Table 2 (e 5.4. Residual solvents).
Solvent solution (c) Dissolve 1.00 g of the solvent or solvents prent in the substance
to be examined in dimethyl sulphoxide R or water R, if appropriate, and dilute to 100.0 ml with water R. Dilute to give a concentration of 1/20 of the limit(s) stated in Table 1 or 2 (e 5.4. Residual solvents).
Blank solution Prepare as described for solvent solution (c) but without the addition of solvent(s) (ud to verify the abnce of interfering peaks).
Test solution Introduce 5.0 ml of the sample solution and 1.0 ml of the blank solution into an injection vial.
Reference solution (a) (Class 1) Introduce 1.0 ml of solvent solution (a) and 5.0 ml of the appropriate diluent into an injection vial.
Reference solution (a1) (Class 1) Introduce 5.0 ml of the sample solution and 1.0 ml of solvent solution (a) into an injection vial.
Reference solution (b) (Class 2) Introduce 1.0 ml of solvent solution (b) and 5.0 ml of the appropriate diluent into an injection vial.
Reference solution (c) Introduce 5.0 ml of the sample solution and 1.0 ml of solvent solution (c) into
an injection vial.
Reference solution (d) Introduce 1.0 ml of the blank solution and 5.0 ml of the appropriate diluent into an injection vial.
Clo the vials with a tight rubber membrane stopper coated with polytetrafluoroethylene and cure with an aluminium crimped cap. Shake to obtain a homogeneous solution.
The following static head-space injection conditions may be ud:
The chromatographic procedure may be carried out using:
System A
—a fud-silica capillary or wide-bore column 30 m long and 0.32 mm or 0.53 mm in internal diameter coated with cross-linked 6 per cent polycyanopropylphenylsiloxane and 94 per cent polydimethylsiloxane (film thickness: 1.8 µm or 3 µm),
—nitrogen for chromatography R or helium for chromatography R as the carrier gas, split ratio 1:5 with a linear velocity of about 35 cm/s,
—a flame-ionisation detector (a mass spectrometer may also be ud or an
electron-capture detector for the chlorinated residual solvents of Class 1),
maintaining the temperature of the column at 40 °C for 20 min, then raising the temperature at a rate of 10 °C per min to 240 °C and maintaining it at 240 °C for 20 min and maintaining the temperature of the injection port at 140 °C and that of the detector at 250 °C, or, where there is interference from the matrix, u:
System B
—a fud-silica capillary or wide-bore column 30 m long and 0.32 mm or 0.53 mm in internal diameter coated with macrogol 20 000 R(film thickness: 0.25 µm),
—nitrogen for chromatography R or helium for chromatography R as the carrier gas, split ratio 1:5 with a linear velocity of about 35 cm/s.
—a flame-ionisation detector (a mass spectrophotometer may also be ud or an
electron-capture detector for the chlorinated residual solvents of Class 1),
maintaining the temperature of the column at 50 °C for 20 min, then raising the temperature at a rate of 6 °C per min to 165 °C and maintaining it at 165 °C for 20 min and maintaining the temperature of the injection port at 140 °C and that of the detector at 250 °C.
Inject 1 ml of the gaous pha of reference solution (a) onto the column described in System A and record the chromatogram under such conditions that the signal-to-noi ratio for 1,1,1-trichloroethane can be measured. The signal-to-noi ratio must be at least five. A typical chromatogram is shown in Figure 2.4.24.-1.
