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2 protocols using potassium hydroxide titrisol

1

Norfloxacin Dissolution Rate Determination

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Norfloxacin (>98%), resorcinol (>99%), and toluene (>99.5%) were purchased from Sigma Aldrich (Darmastadt, Germany). Norfloxacin was a mixture of polymorph A, polymorph C, and the sesquihydrate Form I (Ref Code PUZGAT). See Figure S1 for further details [31 (link)].
The following chemicals were used to prepare buffer solutions: ethylenediamine (>98.8%) from J. T. Baker (Radnor, PA, USA), and trifluoroacetic acid (>99%) and acetic acid (>99%) from Merck (Darmastadt, Germany). To reach the desired pH value, 1 M sodium hydroxide Titrisol® or 0.5 M hydrochloric acid Titrisol®, also from Merck, were added.
For the dissolution rate determination, the following reagents were used: dimethyl sulfoxide (>99.9%, DMSO), potassium dihydrogen phosphate (>99.5%), 0.5 M potassium hydroxide Titrisol®, and 0.5 M hydrochloric acid Titrisol®, all from Merck. Potassium chloride (>99%) was from Sigma.
For HPLC quantification, acetonitrile (HPLC gradient-grade) from Fisher Scientific (Hampton, NH, USA) and a mixture of sodium dihydrogen phosphate monohydrate (>99%) and disodium monohydrogen phosphate (>99%) from Merck were used.
Water was purified by a Milli-Q plus system from Millipore (Bedford, MA, USA), with a resistivity of 18.2 MΩ cm.
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2

Detailed Chemical Characterization Protocol

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Bupivacaine hydrochloride (99%), haloperidol (>98%), lidocaine (>98%), maprotiline hydrochloride (>99%), mifepristone (>98%), and cyproheptadine hydrochloride (99%) were obtained from Sigma-Aldrich (St. Louis, MO, USA).
The following chemicals were used to prepare buffer solutions: acetic acid (>99%), formic acid (98%), and ethylenediamine (>98.8) from J. T. Baker (Center Valley, PA, USA), ammonia solution (25%) and trifluoroacetic acid (>99%) from Merck (Darmstadt, Germany), and ammonium bicarbonate (>99%) from Fluka (Buchs, Switzerland). To reach the desired pH value, 1 M sodium hydroxide or hydrochloric acid were added. The ionic strength of all buffer solutions was fixed to 0.1 M. These reagents were used for pK a determination: dimethyl sulfoxide >99.9% (DMSO), potassium dihydrogen phosphate (>99.5%), 0.5 M potassium hydroxide Titrisol  and 0.5 M hydrochloric acid Titrisol  from Merck. Potassium chloride >99% was from Sigma.
For HPLC quantification, formic acid, sodium formate (>99%, Fluka), and methanol (HPLC gradient grade) from Fisher Scientific (Loughborough, UK) were used.
Water was purified by a Milli-Q plus system from Millipore (Bedford, MA, USA), with a resistivity of 18.2 MΩ cm.
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