Amitriptyline, separation

Note Derivatization with this reagent sequence in combination with extraction and TLC separation is speciftc for amitriptyline and nortriptyline in the analysis of plasma furthermore its high sensitivity allows its employment in pharmacokinetic studies, e. g. after the oral administration of a single dose of 25 mg amitriptyline. 

Fi re 4.15 Separation of the tricyclic antidepressant amitriptyline and its major metabolites on a 10 cm x 4.6 mm I. D. column packed with Spherisorb S5H silica with methanol-aqueous ammonium acetate (9 1), pH 9.1, as mobile phase at a flow rate of about 1 ml/min. Peak identification 1 > amitriptyline-N-oxide 2 amitriptyline 3 - E-lO-hydroxyamitriptyline 4 - Z-10-hyroxyamitriptyline 5 desmethylnortrlptyline 6 nortriptyline 7 E-lO-hydroxynortriptyline and 8 - Z-lO-hydroxynortriptyline. (Reproduced with permission from ref. 271. Copyright Elsevier Scientific Publishing Co.)... 

FIGURE 2.4 Separation of strong bases on a classical RP and on a shielded phase. Columns Prontosil CIS H Prontosil CIS ace EPS (150x4.0mm). Mobile phase MeOH/phosphate buffer 20mM pH=7, 65/35 v/v, 40°C. Analytes 1, uracil 2, protriptyline 3, nortriptyline 4, doxepine 5, imipramine 6, amitriptyline 7, trimipramine S, clomipramine. 

A first study with separate and combined use of IPT and antidepressants (Weissman et al. 1979) comprised 81 outpatients (12 men, 69 women) aged 18 65 years (mean approximately 30 years) suffering from moderate severe unipolar depressions and classified as neurotic depressions. Half of the patients received at least one session of 50 min of IPT per week for 16 weeks the other patients were given the name and telephone number of a psychiatrist at the clinic and could call him whenever they wanted to make an appointment. They were granted a maximum of one therapy session per month. Half of each of the two psychotherapy groups received amitriptyline in individually adjusted daily doses of between 100 and 200mg, or placebo. 

Figure 1.29. LC separation of (1) norephedrine, (2) nortriptyline, (3) toluene, (4) imipnamine, and (5) amitriptyline using columns with various bonded phases [all-ACE column 250mmx4.6mm, 5 pm mobile phase 80/20 (v/v) methanol-25 mM phosphate buffer usually, phosphate buffers are not preferred for MS applications], (Reprinted with permission from Dolan, 2007.)...

Figure 7.5 Typical SFC separation of chlordiazepoxide (1) and amitriptyline hydrochloride (2) on a SB-cyanopropyl-50 column. (From Ref. 4.)...

Berger and Wilson also reported the separation of 10 antidepressants (amitriptyline, imipramine, nortriptyline, desipramine, protripyline, bucliz-ine, benactyzine, hydroxyzine, perphenazine, and thioridazine) using a packed-column SFC with a tertiary mobile phase [37], A Lichrosphere cyanopropyl column with a mobile phase consisting of supercritical fluid carbon dioxide with 10% modifier (methanol with 0.5% isopropylamine) was used for the separation. It was noted that solutes did not elute without the addition of isopropylamine. Detection limits obtained were as low as 88 ppb for a 5-jul injection. 

Spherisorb propyl SCX (3 pm) Spherisorb phenyl SCX (3 pm) Symmetry SCX (3 pm) Spherisrob Mixed Mode (3 pm) Evaluation of various SCX phases, compariosn of electroosomotic mobility at various pHs, separation of antidepressants, amitriptyline, nortriptyline, neutral test mixture MeCN-50 mM phosphate 70 30, pH 2.3 MeCN-20 mM borate 70 30, pH 9.0 [97]... 

Figure 18-5. The separation of therapeutic tricyclic antidepressants on PBD-coated zirconia at different temperatures. Solutes 1, lidnocaine 2, quinidine 3, norephedrine 4, tryptamine 5, amitriptyline 6, nortriptyline. (Reproduced from reference 52, with permission. Copyright 1997, American Chemical Society.)...

Fig. 9 Separation of neutral and basic compounds by electrochromatography thiourea (1), dimethyl phthalate (2), anisole (3), naphthalene (4), nortiptyline (5), amitriptyline (6), clomipramine (7). (For details of experimental conditions, see Ref. 358.)...

Kiel, J.S. Abramson, R.K. Smith, C.S. Morgan, S.L. Development of a rapid extraction and high-performance liquid chromatographic separation for amitriptyline and six biological metabolites. J.Chromatogr., 1986, 383, 119-127... 

Piperaki, S. Parissi-Poulou, M. Koupparis, M. A separation study of tricyclic antidepressant drugs by HPLC with (3-cyclodextrin bonded stationary phase. J.Liq.Chromatogr., 1993, 16, 3487—3508 [also amitriptyline, chloripramine, doxepin, imipramine, maprotiline, protriptyline]... 

Tricyclic antidepressants were analyzed by Vallano et al. [179] via an MIP-CEC separation. In this separation, doxepin, imipramine, amitriptyline, trimipramine, and clomipramine were separated from the template molecule nortriptyline (Figure 5.22). The capillary inner diameter and total length were 100 pm and 33 cm, respectively, and the total length of the monolithic bed was 22.5 cm. The eluent was 92 2 ACN 10 mM sodium acetate pH 3.0 to which 0.02% trifluoracetic acid and 0.015% triethylamine (TEA) (v/v) was added. A constant applied voltage of 30 kV was utilized. 

You are required to separate amitriptyline and nortriptyline using HPLC (chemical structures shown here). 

Po and Irwin (1979) used TLC to separate numerous tricyclic neuroleptic tranquilizers. Samples were dissolved in ethyl acetate, and the mobile phase consisted of mixtures of different n-alcohols with water. Circular development in a Camag U chamber was used, and spots were detected by fluorescence quenching. The /Jp values of some of the better known drugs developed in methanol-water (90 10) were amitriptyline, 0.17 clopenthixol, 0.40 doxepin, 0.42 nortriptyline, 0.37 and promazine, 0.14. Shirke et al. (1994) determined amitriptyline and chlordiazepoxide in combined dosage forms using ethyl acetate-methanol-dieth-ylamine (9.5 0.5 0.05) mobile phase and scanning at 245 nm. 

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