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A New Microchemical Outside Indicator for the Anthraquinone Derivatives†
SCIENTIFIC EDITION Clinically, over 2,500,000 thyroid tablets manufactured from Formula No, 9 have been used in the University of Illinois Hospitals and dispensed through the hospital pharmacy with completely satisfactory results.
SUMMARY
Twelve trial formulas for 65-mg. thyroid tablets are presented. Dried starch and dried bentonite are compared as disintegrants. The dry breaking weights and wet breaking times of the 12 formulas are plotted in comparison with the values of a commercial tablet and the formula previously used at the University of Illinois Manufacturing Pharmacy Laboratory. A formula for 65-mg. thyroid tablets contain-
65 1
ing bentonite as a filler and a disintegrant is presented as having been produced with good results at the University of Illinois Manufacturing Pharmacy Laboratory on a semicommercial scale. A device for measuring the relative disintegration time of compressed tablets is described, and working plans of its construction are given in detail. The method for determining the relative disintegration time is thoroughly discussed. REFERENCES (1) Silver, J. $., and Clarkson R., “Manufacture of Compressed Tablets, ed. 1, F. J. StAkes Machine Co., Philadelphia, Pa., 1944, pp. 3, 35. (2) Berry, H . , Pharm. J . , 143, 174(1939). (3) Thompson, H. O., and Lee, C. O., THIS JOURNAL, 34 138( 1945).
A New Microchemical Outside Indicator for the Anthraquinone Derivatives*’? By BERNARD V. CHRISTENSENS and ISMAIL A. ABDEL-LATIFg T h e red color developed by the alkalies with the anthraquinone derivatives is used as an outside indicator for their detection i n any solution or extract. T h e test is extremely sensitive and the colors obtained are quite stable. HE USE OF solid potassium hydroxide or other solid alkalies as an outside indicator was tried as a means for the detection of the presence or absence of anthraquinone derivatives in any solution or extract, whatever the solvent might be.
T
EXPERIMENTAL Procedure.-A drop of the extract t o be tested was taken out and added t o a pellet of pure potassium hydroxide on a spot plate. A red color developed immediately if any trace of the anthraquinone derivatives existed. Results were always checked with blanks and control experiments. I n cases where solutions in organic solvents were tested, the color developed in a few seconds after the
*
Received Aoril 4. 1949. from the Pharmacoanosv Research- Laborat&, College’of Pharmacy, The 6hio -State University, Columbus, Ohio. Presented to the Scientific Section, A. PH. A., Jacksonville meeting April 1949. t Absjract bf dissertation submitted to the Graduate School bv 1. A. Abdel-Latif in partial fulfillment of the requirements for the degree of Doctor of Philosophy. 1: Dean of the College of Pharmacy, The Ohio State University. 5 Former lecturer, Pharmacognosy Dept., College of Pharmacy, Fouad I Univ., Cario, Egypt. Former Instructor of Pharmacognosy, College of Pharmacy, The Ohio State University.
organic solvent volatilized. The color developed faster with ether than with chloroform and very slowly in case of amyl alcohol. In the case of slowly evaporating organic solvents, it was found advantageous t o warm the solution on the spot plate, on a steam bath, then add a drop of water t o the residue, followed by a pellet of potassium hydroxide. The test was also successful using sodium hydroxide pellets, borax, and sodium bicarbonate. Potassium and sodium hydroxides gave much better results than the other alkalies, which in some instances did not develop the color until a drop of water was added. This may be explained by the fact that the caustic alkalies are deliquescent. Sensitivity.-The test is sensitive to dilutions as high as 0.00002 Gm. senna extractive per drop of extract, or a t least t o ‘/~W,OOO dilution of anthraquinone derivatives. Advantages of the Outside Indicator.-The advantages of this indicator are: ( a ) applicability t o all types of solutions or extracts of the anthraquinone derivatives regardless of the solvent; (b) time- and equipment-saving; ( c ) usefulness in quantitative extractions of emodin-containing drugs; ( d ) it is extremely sensitive and specific; and (e) the colors as well as the fluorescence are stable for a t least twentyfour hours.
SUMMARY
Potassium hydroxide pellets are recommended to be used as an outside indicator for the detection of traces of anthraquinone derivatives in any extract of the emodin drugs or as a solution thereof, whatever the solvent may be.
SUMMARY
Twelve trial formulas for 65-mg. thyroid tablets are presented. Dried starch and dried bentonite are compared as disintegrants. The dry breaking weights and wet breaking times of the 12 formulas are plotted in comparison with the values of a commercial tablet and the formula previously used at the University of Illinois Manufacturing Pharmacy Laboratory. A formula for 65-mg. thyroid tablets contain-
65 1
ing bentonite as a filler and a disintegrant is presented as having been produced with good results at the University of Illinois Manufacturing Pharmacy Laboratory on a semicommercial scale. A device for measuring the relative disintegration time of compressed tablets is described, and working plans of its construction are given in detail. The method for determining the relative disintegration time is thoroughly discussed. REFERENCES (1) Silver, J. $., and Clarkson R., “Manufacture of Compressed Tablets, ed. 1, F. J. StAkes Machine Co., Philadelphia, Pa., 1944, pp. 3, 35. (2) Berry, H . , Pharm. J . , 143, 174(1939). (3) Thompson, H. O., and Lee, C. O., THIS JOURNAL, 34 138( 1945).
A New Microchemical Outside Indicator for the Anthraquinone Derivatives*’? By BERNARD V. CHRISTENSENS and ISMAIL A. ABDEL-LATIFg T h e red color developed by the alkalies with the anthraquinone derivatives is used as an outside indicator for their detection i n any solution or extract. T h e test is extremely sensitive and the colors obtained are quite stable. HE USE OF solid potassium hydroxide or other solid alkalies as an outside indicator was tried as a means for the detection of the presence or absence of anthraquinone derivatives in any solution or extract, whatever the solvent might be.
T
EXPERIMENTAL Procedure.-A drop of the extract t o be tested was taken out and added t o a pellet of pure potassium hydroxide on a spot plate. A red color developed immediately if any trace of the anthraquinone derivatives existed. Results were always checked with blanks and control experiments. I n cases where solutions in organic solvents were tested, the color developed in a few seconds after the
*
Received Aoril 4. 1949. from the Pharmacoanosv Research- Laborat&, College’of Pharmacy, The 6hio -State University, Columbus, Ohio. Presented to the Scientific Section, A. PH. A., Jacksonville meeting April 1949. t Absjract bf dissertation submitted to the Graduate School bv 1. A. Abdel-Latif in partial fulfillment of the requirements for the degree of Doctor of Philosophy. 1: Dean of the College of Pharmacy, The Ohio State University. 5 Former lecturer, Pharmacognosy Dept., College of Pharmacy, Fouad I Univ., Cario, Egypt. Former Instructor of Pharmacognosy, College of Pharmacy, The Ohio State University.
organic solvent volatilized. The color developed faster with ether than with chloroform and very slowly in case of amyl alcohol. In the case of slowly evaporating organic solvents, it was found advantageous t o warm the solution on the spot plate, on a steam bath, then add a drop of water t o the residue, followed by a pellet of potassium hydroxide. The test was also successful using sodium hydroxide pellets, borax, and sodium bicarbonate. Potassium and sodium hydroxides gave much better results than the other alkalies, which in some instances did not develop the color until a drop of water was added. This may be explained by the fact that the caustic alkalies are deliquescent. Sensitivity.-The test is sensitive to dilutions as high as 0.00002 Gm. senna extractive per drop of extract, or a t least t o ‘/~W,OOO dilution of anthraquinone derivatives. Advantages of the Outside Indicator.-The advantages of this indicator are: ( a ) applicability t o all types of solutions or extracts of the anthraquinone derivatives regardless of the solvent; (b) time- and equipment-saving; ( c ) usefulness in quantitative extractions of emodin-containing drugs; ( d ) it is extremely sensitive and specific; and (e) the colors as well as the fluorescence are stable for a t least twentyfour hours.
SUMMARY
Potassium hydroxide pellets are recommended to be used as an outside indicator for the detection of traces of anthraquinone derivatives in any extract of the emodin drugs or as a solution thereof, whatever the solvent may be.