Ipecac Oral Solution
Monograph under this new title—to become official June 1,2005
(Current monograph title is Ipecac Syrup)
»Ipecac Oral Solution yields,from each 100mL,not less than 123mg and not more than 157mg of the total ether-soluble alkaloids of ipecac.
The content of emetine (C29H40N2O4)and cephaeline (C28H38N2O4)together is not less than 90.0percent of the amount of the total ether-soluble alkaloids.The content of cephaeline varies from an amount equal to,to an amount not more than 2.5times,the content of emetine.
| Powdered Ipecac | 70g |
| Glycerin | 100mL |
| Syrup,a sufficient quantity,to make | 1000mL |
Exhaust the powdered Ipecac by percolation,using a mixture of 3volumes of alcohol and 1volume of water as the menstruum,macerating for 72hours,and percolating slowly.Reduce the entire percolate to a volume of 70mLby evaporation at a temperature not exceeding 60
and preferably in vacuum,and add 140mLof water.Allow the mixture to stand overnight,filter,and wash the residue on the filter with water.Evaporate the filtrate and washings to 40mL,and to this add 2.5mLof hydrochloric acid and 20mLof alcohol,mix,and filter.Wash the filter with a mixture of 30volumes of alcohol,3.5volumes of hydrochloric acid,and 66.5volumes of water,using a volume sufficient to produce 70mLof the filtrate.Add 100mLof Glycerin and enough Syrup to make the product measure 1000mL,and mix.
and preferably in vacuum,and add 140mLof water.Allow the mixture to stand overnight,filter,and wash the residue on the filter with water.Evaporate the filtrate and washings to 40mL,and to this add 2.5mLof hydrochloric acid and 20mLof alcohol,mix,and filter.Wash the filter with a mixture of 30volumes of alcohol,3.5volumes of hydrochloric acid,and 66.5volumes of water,using a volume sufficient to produce 70mLof the filtrate.Add 100mLof Glycerin and enough Syrup to make the product measure 1000mL,and mix.
Packaging and storage—
Preserve in tight containers,preferably at a temperature not exceeding 25.Containers intended for sale to the public without prescription contain not more than 30mLof Oral Solution.
.Containers intended for sale to the public without prescription contain not more than 30mLof Oral Solution.
Microbial limits á61ñ—
It meets the requirements of the tests for absence of Escherichia coli.
Assay for total ether-soluble alkaloids—
[NOTE—It is important that the ether used in this assay shall have been shown by test to be free from peroxides within 24hours prior to use.]Transfer about 50mL,accurately measured,of Oral Solution to a liquid-liquid automatic extractor,add water,if necessary,to reduce the viscosity,render the liquid distinctly alkaline with ammonium hydroxide,and extract with ether for at least 4hours or until the extraction is complete.Use a water bath to boil the ether.Frequently disconnect the extractor from the condenser,and agitate the lower layer by raising and lowering the center tube or by other suitable manipulation.At the conclusion of the extraction period,transfer the ether extract to a separator,and rinse the extraction flask with 2or more small volumes of ether,adding the rinsings to the separator.Complete the assay as directed in the Assay for total ether-soluble alkaloidsunder Ipecac,beginning with “Extract the alkaloids from the ether.”
Assay for emetine and cephaeline—
Standard preparation,Phosphate buffer,andCitric acid buffer—
Prepare as directed in the Assay for emetine and cephaelineunder Ipecac.
Assay preparation—
Pipet 10mLof water into a 25-mLvolumetric flask.With the aid of a 20-mLpipet,add Oral Solution to volume,taking care to prevent contact of the Oral Solution with the neck of the flask above the graduation line.Insert the stopper,and mix.
Chromatographic columns—
Pack a pledget of fine glass wool in the base of a chromatographic tube (25-mm ×200-mm test tube to which is fused a 5-cm length of 7-mm tubing)with the aid of a tamping rod having a disk with a diameter about 1mm less than that of the tube.
To prepare Column I,transfer 4.0mLof the Assay preparationto a 150-mLbeaker,add about 1g of sodium bicarbonate,and mix.Then proceed as directed for Chromatographic columnsin the Assay for emetine and cephaelineunder Ipecac,beginning with “add 6g of purified siliceous earth,”and prepare Columns II,III,and IVas directed therein.
Procedure—
Proceed as directed for Procedurein the Assay for emetine and cephaelineunder Ipecac.
Calculate the quantity,in mg,of emetine in each 100mLof Oral Solution taken by the formula:
2.08C(A283-A350)U/(A283-A350)S,
in which the parenthetic expressions are the differences in the absorbances of the solution of emetine from the Assay preparation(U)and the Standard preparation(S),respectively,at the wavelengths indicated by the subscripts,and Cis as defined in the Procedure.
Calculate the quantity,in mg,of cephaeline in each 100mLof Oral Solution taken by the formula:
0.971(2.08C)(A283-A350)U/(A283-A350)S,
in which 0.971is the ratio of the molecular weight of cephaeline to that of emetine,the parenthetic expressions are the differences in the absorbances of the solution of cephaeline from the Assay preparation(U)and the Standard preparation(S),respectively,at the wavelengths indicated by the subscripts,and Cis as defined in the Procedure.
(Official June 1,2005)
Auxiliary Information—
Staff Liaison:Gabriel I.Giancaspro,Ph.D.,Senior Scientist and Latin American Specialist
Expert Committee:(DSB)Dietary Supplements:Botanicals
USP28–NF23Page 1061
Pharmacopeial Forum:Volume No.28(2)Page 310
Phone Number:1-301-816-8343