General Tests, Processes and Apparatus - mfds.go.kr

1 General tests , Processes and Apparatus KP X 1571. General tests , Processes and Apparatus 1. Alcohol Number Determination .. 1573 36. Nuclear Magnetic Resonance 1638. 2. Ammonium Limit Test .. 1574 37. Optical Rotation Determination .. 1640. 3. Arsenic Limit Test .. 1576 38. Osmolarity Determination .. 1641. 4. Atomic Absorption Spectrophotometry .. 1577 39. Oxygen Flask Combustion Method .. 1642. 5. Bacterial Endotoxins Test .. 1578 40. Particle Size Distribution Test for 6. Bioautography .. 1583 Preparations .. 1644. 7. Boiling Point and Distilling Range Test .. 1583 41. pH Determination .. 1644. 8. Chloride Limit Test .. 1584 42. Pyrogen Test .. 1646. 9. Conductivity 1585 43. Qualitative tests .. 1646. 10. Congealing Point Determination .. 1586 44. Readily Carbonizable Substances Test .. 1653. 11. Crystallinity 1587 45. Refractive Index Determination .. 1653. 12. Determination of Specific Gravity and 46. Residue on Ignition Test .. 1653. 1587 47. Sterility Test .. 1654. 13. Determination of Volume of Injection in 48.

2 Sulfate Limit Test .. 1658. Containers .. 1589 49. Test for Acid-neutralizing Capacity .. 1658. 14. Digestion Test .. 1590 50. Test for Glass Containers for Injections .. 1659. 15. Disintegration Test .. 1593 51. Test for Herbal Drugs .. 1660. 16. Dissolution Test .. 1596 52. Test for Histamine .. 1676. 17. End point detection methods in Titrimetry .. 1601 53. Test for Metal Particles .. 1677. 18. Fats and Fatty Oils Test .. 1603 54. Test for Rubber Closure for Aqueous 19. Flame Coloration 1606 Infusions .. 1677. 20. Fluorometry .. 1606 55. Test for Total Organic Carbon .. 1678. 21. Foreign Insoluble Matter Test .. 1606 56. Test Methods for Plastic Containers .. 1680. 22. Gas Chromatography .. 1607 57. Thermal 1685. 23. Heavy Metals Limit Test .. 1611 58. Thin-layer Chromatography .. 1687. 24. Infrared Spectrophotometry .. 1612 59. Ultraviolet-visible Spectrophotometry .. 1688. 25. Insoluble Particulate Matter Test for 60. Uniformity of Dosage Units .. 1689. Injections .. 1613 61. Viscosity Determination.

3 1693. 26. Insoluble Particulate Matter Test for 62. Vitamin A Assay .. 1697. Ophthalmic Solutions .. 1616 63. Water Determination (Karl Fischer Method) .. 1698. 27. Iron Limit Test .. 1617 64. X-Ray Powder Diffraction Method .. 1701. 28. Liquid Chromatography .. 1618 65. Reference Standards; Reagents,Test Solutions;. 29. Loss on Drying Test .. 1619 Standard Solutions for Volumetric Analysis;. 30. Loss on Ignition Test .. 1620 Standard Solutions;Matching Fluids for Color;. 31. Melting Point Determination .. 1620 Optical Filters for Wavelength and Transmission 32. Microbial Assay for Antibiotics .. 1622 Rate Calibration; Measuring Instruments, 33. Microbial Limit Test .. 1627 Appliances; Sterilization and Aseptic 34. Mineral Oil Test .. 1637 Manipulation .. 1706. 35. Nitrogen Determination (Semimicro-Kjeldahl Method) .. 1637. KP X 1573. distilling flask, A, add 5mL of water and boiling chips. 1. Alcohol Number Distil ethanol carefully into the glass-stoppered, volu- Determination metric cylinder, D.

4 By reference to the following Table, a suitable The Alcohol Number represents the number of volume of distillate (mL) should be collected, accord- milliliters of ethanol at 15 C obtained from 10mL of ing to the content of ethanol in the sample preparation. tincture or other preparations containing ethanol by the Prevent bumping during distillation by rendering the following procedures. sample strongly acidic with phosphoric acid or sulfuric acid, or by adding a small amount of paraffin, beeswax Method 1. Distilling method or silicone resin before starting the distillation. When This is a method to determine the Alcohol Num- the samples contain the following substances, carry out ber by reading the number of milliliters of ethanol dis- pretreatment as follows before distillation. tillate at 15 C obtained from 10mL of a sample meas- (i) Glycerin: Add sufficient water to the sample so ured at 15 C by the following procedures. that the residue in the distilling flask, after distillation, (1) Apparatus : Use hard glass Apparatus as illus- contains at least 50 % of water.

5 Trated herein. Ground glass may be used for the joints. (ii) Iodine: Decolorize the sample with zinc pow- (2) Reagent: Alkaline phenolphthalein solution: der. To 1 g of phenolphthalein, add 7mL of sodium hydrox- (iii) Volatile substances: Preparations containing ide TS and water to make 100mL. appreciable proportions of essential oil, chloroform, ether or camphor require treatment as follows. Mix 10mL of the sample, accurately measured, with 10mL. of saturated sodium chloride solution in a separator, add 10mL of petroleum benzin, and shake. Collect the separated aqueous layer. The petroleum benzin layer was extracted with two 5mL volumes of saturated so- dium chloride solution. Combine the aqueous layers, and distill. According to the ethanol content in the sample, collect a volume of distillate 2 to 3mL more than that shown in the below Table. (iv) Other substances: Render preparations con- taining free ammonia slightly acidic with dilute sulfu- ric acid. If volatile acids are present, render the prepa- ration slightly alkaline with sodium hydroxide TS, and if the preparations contain soap along with volatile substances, decompose the soap with an excess of di- lute sulfuric acid before the extraction with petroleum benzin in the treatment described in (iii).

6 To the distil- late, add 4 to 6 g of potassium carbonate and 1 to 2. drops of alkaline phenolphthalein solution, and shake vigorously. If the aqueous layer shows no white turbid- ity, agitate the distillate with additional potassium car- bonate. After allowing to stand in water at 15 2 C. for 30 minutes, read the volume of the upper reddish ethanol layer inmL, and regard it as the Alcohol Num- ber. If there is no clear boundary surface between these two layers, shake vigorously after addition of a few drops of water, then observe in the same manner. Table. Amount of Distillate A: Distilling flask (50mL) Ethanol content in Distillate B: Delivery tube the sample (vol %) to be collected (mL). C: Condenser Above 80 13. D: Glass-stoppered volumetric cylinder (25mL, 80 - 70 12. graduated in ) 70 - 60 11. 60 - 50 10. Figure. Apparatus used or the Alcohol Number 50 - 40 9. Determination. 40 - 30 8. Below 30 7. (3) Procedure: Transfer 10mL of the sample preparation, accurately measured at 15 2 C, to the Method 2.

7 Gas chromatography 1574 General tests , Processes and Apparatus This is a method to determine the Alcohol Num- Selection of column: Proceed with 1mL of the gas ber by determining ethanol (C2H5OH) content (vol %) obtained from the standard solution in the bottle under from a sample measured at l5 C by the following pro- the above operating conditions, and calculate the reso- cedures. lution. Use a column giving elution of ethanol and the (1) Reagent Dehydrated ethanol for Alcohol internal standard in this order with a resolution be- Number: Dehydrated ethanol with determined ethanol tween their peaks being not less than (C2H5OH) content. The relation between specific gravi- ty, d1515 , of dehydrated ethanol and ethanol (C2H5OH). content is : vol %, : vol %, and 2. Ammonium Limit Test vol %. (2) Preparation of test solution and standard so- The Ammonium Limit Test is a limit test for am- lution Test solution -Measure accurately a volume of monium contained in drugs. sample at 15 2 C equivalent to about 5mL of ethanol In the monograph, the permissible limit for am- (C2H5OH), and add water to make exactly 50mL.

8 Monium (as NH4+) is described in terms of percentage Measure accurately 25mL of this solution, add exactly ( %) in parentheses. 10mL of the internal standard solution, and add water to make 100mL. Apparatus Standard solution-Measure accurately 5mL of de- Use a distilling Apparatus for ammonium limit test hydrated ethanol for Alcohol Number at the same tem- as illustrated in Figure 1. For the distillation under re- perature as the sample, and add water to make exactly duced pressure, use the Apparatus shown in Figure 2. 50mL. Measure accurately 25mL of this solution, add Either Apparatus is composed of hard glass, and exactly 10mL of the internal standard solution, and add ground-glass joints may be used. All rubber parts used water to make 100mL. in the Apparatus should be boiled for 10 to 30 minutes (3) Procedure Place 25mL each of the test solu- in sodium hydroxide TS and for 30 to 60 minutes in tion and the standard solution in a 100-mL, water, and finally washed thoroughly with water before narrowmouthed, cylindrical glass bottle sealed tightly use.

9 With a rubber closure and aluminum band, immerse the bottle up to the neck in water, allowed to stand at room Procedure temperature for more than 1 hour in a room with little (1) Preparation of test solution and control solu- change in temperature, shake gently so as not to splash tion Unless otherwise specified, the test solutions and the solution on the closure, and allow to stand for 30 the control solution are prepared as directed in the fol- minutes. Perform the test with 1mL each of the gas in lowing. Place an amount of the sample, directed in the the bottle with a syringe according to the Gas Chroma- monograph, in the distilling flask A. Add 140mL of tography under the following conditions, and calculate water and 2 g of magnesium oxide, and connect the the ratios, QT and QS , of the peak height of ethanol to distillation Apparatus . To the receiver F, add 20mL of that of the internal standard. boric acid solution (1 in 200) as an absorbing solution, and immerse the lower end of the condenser.

10 Adjust Alcohol Number the heating to give a rate of 5 to 7mL per minute of distillate, and distill until the distillate measures 60mL. Q 5 (mL). = T Remove the receiver from the lower end of the conden- QS a volume (mL) of sample ser, rinsing the end part with a small quantity of water, ethanol (C 2 H 5 OH) content (vol%) of add sufficient water to make 100mL and designate it as the test solution. dehydrated ethanol for Alcohol Number . Internal standard solution -A solution of acetoni- trile (3 in 50). Operating conditions Detector: A hydrogen flame-ionization detector. Column: A glass tube, about 3 mm in inside diame- ter and about m in length, packed with 150 m to 180 m porous ethylvinylbenzenedivinylbenzene co- polymer for gas chromatography. Column temperature: A constant temperature be- tween 105 C and 115 C. Carrier gas: Nitrogen. Flow rate: Adjust the flow rate so that the retention time of ethanol is 5 to 10 minutes. KP X 1575. Place a volume of standard ammonium solution, directed in the monograph, in the distillation flask A or the vacuum distillation flask L, proceed as for the preparation of the test solution, and designate it as the control solution.