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Recommended HPLC systems 737 is given above. For systematic toxicological screening of blood (serum, plasma) samples by HPLC-DAD, the measurement of two extracts ‘obtained at pl? and pH! 9 with dichloromethane and ofthe supernatant ‘of s protein precipitation by acctonitrile has proved to be very useful (Pragst et al. 2002) Preparation of a basic and an acidic methylene chloride extract 1. Dispense S004 of whole Blood, serum o¢ plasma into twa 1.S-ml, vial, ‘To vial 1 add 100 iL of a 0.2 mol/L solution of u amine (basic extract. ‘To vial 2 add 10041. of 0.1 mol/L hydrochloric acid (acidic extrac), ‘To both vials add 400 UL. of dichloromethane. Vortex mix the vials for I min and centrifuge. Withdraw 200 ofthe dichloromethane extract and evaporate the solvent at room temperature under a steam of nitrogen, Dissolve the residue in 100 of mobile phase “Analyse SOL ofeach extract (basic extract in mobile phase A and acidic extract in mobile phase B) laydroxymethyl) Protein precipitation by acetonitrile 1. To S00uL of whole blood, serum o plasma add 500 pL of aceto- nitrile 2. Vortex the mixture for 2min and centrifuge. 5. Separate off the supernatant. 44. Analyse 5O4L in mobile phase A. Protein precipitation is particularly useful for hydrophilic drugs, which are extracted poorly by the procedure mentioned above, These inclade paracetamol, salicylic acid and lamotrigine, The limits of detection are between 0.01 and 0.1 g/ml for dichloromethane extraction (depend- ing on the extinction coefficient and on the extraction yield) and Jhetween 0.1 and I pg/ml. for protein precipitation. Application example InSTA, the library search must be applied tall peaks ofthe HPLC-DAD chromatogram, As an example, the chromatogram at 225nm of the basic extract from the blood sample of a lethal drug poisoning case and the UV spectra ofthe highest peaks are shown in Figure 41.14. To determine RAT, the standard compound (MPPH, peak no. 10, RT = 1.000) was added. From the remaining 11 peaks ofthe chrom. atogram, 7 could be identified by both UV spectrum and RRT. As the result a high overdose of rimipramine and promethazine was found to bbe the cause of death, The extensive metabolism indicated that there had ‘been a long survival time after drug ingestion. The similarities between the UV spectra ofthe parent drugs (peaks 9 and 12) and some oftheir metabolites (peak 8, and peaks 6 and 11 respectively) are also demon: strated in this case, On the other hand, the sulfoxide of promethazine (peak 3) and desmethylpromethazine (peak 2) show completely chan- ged spectra because ofthe transformation that takes place directly a the UV absorbing phenothiazine ring. Cafcine (peak 1) is found in almost all samples. The poor separation of peaks 4,3 and 7 meant thatthe UV spectra were not suitable fora brary search Recommended HPLC systems ‘There are general screening methods based on gradient elution and retention indices that have proven value by many laboratories, and data from these are liste below (systems HA, HX, HZ, HYand HAA). ‘Another (system HBK) is based on a combination of isocratic systems. ‘The tabulated data are derived from systems in which groups of compounds have been chromatographed either as part of 2 general screening procedure or from systems that have been used specifically for that group of compounds. Other systems for the chromatography ‘of individual compounds, especially those used for quantification, are tgiven in the monographs Chromatographic retention data are presented ask values as wll as retention times (RTs), retention indices (Rls) and relative retention times (RTS) Note In the tables, a dash indicates that no value is available forthe compound, nat that it doesnot elute General screens ‘System HA Jane er al. (1985), Colum: Silica Spherisor S5W (125 x 4.9mm id, 5 ym). |= Mobile phase: Solution containing 1.175. (0.01 mol/L) ammonium perchlorate in 1 L-methanol adjust to pH 6.7 by the addition of I mL 0.1 mol/L sodium hydroxide in methanol f= values: Values for drags in this system will be found in drug ‘monographs and in the Indexes to Analytical Data; they are also included inthe systems for specific groups of drugs that follow. System HX J Hanstra, JP Franke, RA de Zeeww, personal communi 1 Colum: Lichrospher 60 RP-Selct B(125 x 4.0mm id, 5m) with precolumn Lichrospher 6 RP-Select B (4 x 40mm id, 5m). 1 Mobile phase: (A:B) teethylammonium phosphate buffer (25 mmol! L pH 3.0)-acetonitrile = Elution programme: (A:B) (100:0) to (30:70) in 30min, hold min, back to intial conditions in 3min with equilibration for min before next injection, 1 Flow rate: 1 mL/min 1 Detection: DAD. 1 Standards: Niteo-r-alkanes (C, to C,,) 104 in 10m. acetonitrile [RU values: Values for drugs in this system will be found in the mono- ‘graphs and inthe Indexes to Analytical Data they are also included in the systems for specific groups of drags that follow. System HY RK Watt, RA Waters, AC Motfit, unpublished information, © Colum: Cyy symmetry (250 x 4.6mm id, Sum) ‘= Column temperature: 40°C. 1 Mobile phase: (A:B) sulfuric acid (03m 25 mol) in water (500 ml) -suluric acid (0.5 mL 28 mol/L) in acetonitrile (500 mL). |= Elution programme: (98:2) for 3 min to (2:98) over 23 min, bold for Wimin, back to initial conditions over 2min with equilibration of ‘Simin before next injection Detection: DAD. Standards: Nitro-r-alkanes (C, 0 Cg) UL in 10m. acetonitrile. [RU values: Values for drugs in this system will be found in the monographs and in the Indexes to Analytical Data; they are also included in the systems for specific groups of drugs that follows System HZ ‘Conemans.JMH et al. hutpy/wwwzanob.ol/pages/LSShowElements Page_v2.asp?ListID = 16508elemid =29275Sarticlid 133751 Stoker (accessed 14 December 2010) © Column: Cys end-capped LiChrospher 100 RP-18e (125 4.0mm id, Sum), with precolumn LiChrocart 124-4 "= Mobile phase: Add 1464L triethylamine and about 750 tL. phos- pphoric acid 10530 mL water. Adjust pH to 3.3 using a 10% potassium hydroxide solution and finally add 470 ml. acetone © Flow rate: 0.6 mL/min. Detection: DAD. [Retention times: Values for drugs in this system will be found in the monographs and in the Indexes to Analytical Data; they are also included in the systems for specific groups of drugs that follows System HAA Gaillard ¥, Pepin G. (1997). J Chromatogr A 763: 149-163. © Colum: Cy Symmetry (250 x 4.6mm id, 5 am) with Symmetry Cie precoluma (20 mm). Column temperature: 30°C, Mobile phase: (AB) phosphate buffer (pH 3.8)-acetonitile 1 Elution programme: (85:15) for 6 min to (65:38) until 25 min to (20:80) for 3 min, and back to initial conditions for equilibration for 7 min, 738 High Performance Liquid Chromatography 10 [P Ga 225 om 50 ‘Absorption (mAbs) " 2 5 PaaS Promethazine-S-oxide oa al\ | rmelabote SVN 1 il Bl =f. a0 aT on Benue We nae at Peak 2 Thimipremine | AP ugimt \Wavelenath (om) Figure 41.14 | HPLC-DAD investigation ofa combined timipramine-promethazine poisoning. Chromatogram of abasic extract ofa venous blood sample, UY Specta ofthe nighest peaks, results ofthe library serch end semiquantitatwely determined concentrations slow rate:1 mL/min for 6.5 min, then line for 6.5-25min and hold for 3min (re-equilibration is made at LSmi/min), = Detection: DAD. increase to 1.5 mL/min = Retention times: Values for drugs in this system will be found in the monographs and in the Indexes to Analytical Data; they are also included in the systems for specific groups of drugs that follove Recommended HPLC systems 739 ‘System HBK Pragst Ft al. (2001) UV Spectra of Taxie Verlag Dr Dieter Helm, |= Column: Lichrospher RP-8ec (250 x 4.0mm id, 5 4m). "= Mobile phase: Three different composition are used: A: acetoni- trile-phosphate buffer pH 2.3 (33267). Internal standard: 5-(4- methyipheny!)-5-phenylhydantoin (for compounds eluting within 30 min). B: acetonitrile-phosphate buffer pH 2.3 (67233). Internal standard: 4-phenylbenzophenone (for compounds eluting after 30min). Ci acetonitrile-phosphate butler pH 23 (20:80) Internal standard: salicylamide (for compounds with RRTS below 02). low rate: V mL/min, Detection: DAD. ‘a Note: The phosphate butte is prepared by dissolving 4.8 g phospho- ric acid (85%) and 6.66 potassium dihydrogenphosphate in IL ‘water, adjust pH to 2.3. Values for drugs inthis system will only be found in the Indexes to Analytical Data ‘ompounds. Heppenkeim: Amfetamines, other stimulants and anorectics Systems HA, HX or HY previously described may be used, oF Systems HB or HC below. ‘System HB {Gi R er al. (1981). J Chromatogr 218: 639-646, Colum: ODS Hypersil (250 x 5mm id, 5 um). = Mobile phase: Solution containing 19.60 (0.2 mol/L) phosphoric acid and 7.314 (0.1 mol/L) diethylamine in 1 of a 10% viv solu- tion of methanol; adjust the pH to 3.15 by the addition of sodium hydroxide solution ‘System HC Law Bt al. (1984). J Chromatogr 301: 165-172, = Column Silica Spherisorb (250 x 5mm id, 5m). |= Mobile phase: Methanol-ammonium nitrate buffer solution (90:10), To prepare the bufler solution add 9 mi. strong ammonia solution and 21.5 mL nitric acid to 884 ml. water and adjust to pH 10 by the {addition of strong ammonia solution, ‘Amfetamines, other stimulants and anorectics ry 48 HC HX HY © % % a @ Rarenatne = 06 Amfetamine 09 248 098 28 - Bensfetamine 12 - ous - - Brucine m - - a2 267 afeine 02 - 026 - - Gathine 1 439 oa - - Chlerphentermine 09 - oa - - Diethylpropion Ww - 016 - 230 Dimethylamfetamine - M08 189 - - Dom - - 1a - - Ephedrine 10 568 179 - - Fencamfamin 13 - o72 a4 309 Fenethyline - - 027 - - Fenfluramine 13 - 08a ant as Nocenfuramine 1 - - - - Fenpropores - - - - 226 Hordenine - 200 - - - Hydrnyamfetamine - 224 a - - Hydroyephedrine - o7a - - - Mazin! 18 - 02 as7 286 Mephentermine 18 - 248 - - Mescalne 13 1682 217 - - Metamfetamine 2 10s2 207 262 216 Methoxyamfetamine - 1495 - - - Methoxyphenamine Ww 3217 - - - Methylamfetamine 20 1052 207 - - Methyieneciaaymethamfetamine - - - 278 2s2 Methylephedrine 23 - 13 - - Methyiphenidate W - 036 - ead Noradrenaline - 010 - - - Normetanephrine - - 108 - - oxecrine - 027 - - - Pemoline 02 - on 307 an Phendimetazine 09 - 03 263 28 Pheneltine 10 sar 037 - - ‘ontid 740 High Performance Liquid Chromatography Phenetiylamine 12 364 Ta Phenmetraine W - - 258 2a Phentermine os 1946 08s - 24s Phenylephrine 13 - 168 - - Penypropanolamine 09 387 070 - - Pipradeo! 2 - 069 355 - Pralintane 2 - a 370 - Pseudoephedrine 2 590 Ww - - “Tranyleypromine 10 - 026 - - ‘Tiimethoxyamfetamine - - 148. - - Tyeamine 2 ost 147. - - Analgesics, non-steroidal anti-inflammatory drugs Antifungals System HD The general screening systems, previously described, may be used. HM Stevens, R Gill, unpublished data © Column: ODS Hypersi (160 5 mm id, 5 um). 1 Mobile phase Isypropylalcohol-tormic scid-0.1 mol/L, potassium [EXSR = dlihydrogenphosphate (18.61 giL; 540: 1: 1000) ca HY Hz. HAA ‘System HV mr ar ar ar 2 Column: ODS Spherisorb (200 x 4.6mm ily 5m). sss 1 Mobile phase: Acetronitrile-acetic acid (45:53) for2min, to (75:25) Feonazale 526 385 201 at 386/min, for min, Fuconamole 340 289 - na sa Flow rate: 1.7 maim Fucytosine 72 - 18 a1 ‘System HW Griseofuiin 498 - 184 HM Stevens, R Gill, unpublished data Ketoconazole 439 464 52 157 |= Column: As for System HD, above. |= Mobile phase: Isapropyl alcohol-formic acid-0.1 mol/L. potassium dihydrogenphosphate (18.61 giL; 17621: 1000) 4D WV AW HK HY HZ HAA % PRT xe @ ® ar ca Teeaniide 0S = 2 aT Paracetamol 01 - 032 - - - - Alcofenae 26 os - - - - - ‘Aminophenazone 02 - 032 262 208 2a - Aspicin os: - 27 350 a8 27 - Salicylic ac 07 - 46 - - - - Benoit o7 - 224 - - - - Aspirin os - 27 - - - - Paracetamol on - 032 - - - - Benoxaprofen m3 ose - - - - - loin - 087 - - 24s - - Diclofenac us as. - ois soz 148 2A ifunisl 4 077 - 508 sea 54 - Dipyrone on - 04s, 316 194 14 - xenzamide oss - 46 - 303 - - Fenbufen 4 oat - 520 461 - 193 Fenoprofen 79 - - s7a 524 109 22 Floctafenine - - - - - 44 172 Fufenamic acid 197 1 - on 667 - - Funixin - 099 - - a4 - - Recommended HPLC systems 741 = a : ea fi fn ar nace the pent reigns ev esc, may be sed a irene ome es "amoxelin 225 31 incline ° xo 26 Tans 742 High Performance Liquid Chromatography The general screening systems, previously described, may be wsed oF systems HAX and HAY belo. ‘System HAX Koves EM (1995). J Chromarogr 692: 103-119. © Column: Supelcosil LC-DP (250 x 446mm id, Sym). sm Eluent: (A:B:C) Acetontele-phosphoric acid (0.025% vv)~ triethylamine bute. Isocratic elution: (25: 10:5). lowe eat: 0,6 mL/min, Detection: DAD (2. 229 nm). (te: The triethylamine (TEA) bulfer is prepared by adding 9 ml concentrated phosphoricaci and 10 mLTEA to 900 ml. water, adjusted to pH 3.4 with diluted phosphoric acid and made p to I L with water ‘System HAY Koves EM (1995). J Chromatogr A 692: 103-119. |= Column: LiChrospher 100 RP-8 (250 x 4.0mm id, 5 ym) © luent:(A:1:C) as for System HAX. 1 Iscratic elution: (60:28:15) 1 Flow rate 06mm © Detection: DAD (2.5229 nm) ‘Anticonvulsants and barbiturates System HE (Christofides JA, Fry DE (1980). Clin Chem 26: 499-501 "© Colum: Alkylslica SAS-Hypersil (125 x 45mm id, Sum) = Mobile phase: Acctontrle-tetrabutylammonium’ — phosphate, (0.005 mol/L, pH 7.5 (20:80). System HG GIL Rt al. (1981). J Chromatogr 204: 275-284, Column: ODS Hypersil (150 x-4.6mm id, 5 um). = Mobile phase: Methanol-0.1 mol/L sodium dihydrogenphosphate (11.998 g/L) (40:60); adjust to pH 3.5 by the addition of phosphoric sci, System HH Gill Ret al. (1981). J Chromatogr 226; Biomed Appl 15: 117-123 1 Column: As for System HG, above. = Mobile phase: As for System HG except that the mixture is adjusted to pH 85 by the addition of sodium hydroxide solution HA Wx HY HZ HAA AX Hay k Rr Rr ar ar ar ar ‘aiphenine TS TE = = - = Aropine 39 306 21 22 104 7 38. Biperiden - - - 64 148 - - Chlerphenosamine 29 - 346 - - - - iim - 379 - - - - - Cldinumn bromide - - - - 133 - - Cycopentolate 16 353 287 32 - - - Dicyloverine u - S75 - - - - Diethasne a4 - - - - 151 74 Emepronium bromide 52 420 - - - - - Homatopine a2 2 223 - - 68 a6 Hyoscine uu 270 253 - 74 7 ay Hyoscyamine a7 - - - 97 - : Isopropamide lide 24 379 - - - - - Metixene 36 451 - - - - . Orphenadtine 3 413 aa 6 - - - NeMonodesmethylorphenadsine 17 - - - - - . N-Oxide a - - - - - - wyphencyctimine 28 424 - - - - - Cxyphenenium bromide 26 424 - - - - - Pipedolate wv 429 - - - - - Procytidine 2 405 - 62 - 220 47 Profenamine 24 a6 238 - - 166 83 Propantheine bromide 44 486 - - - - - anthanoi aid - 499 - - - - - Tahesypheniy! 18 429 381 76 153 - - Recommended HPLC systems 743 WK ay HZ « k ® RL ar ibaa Tas Ts ue a amobarbital 1091 708 428 ara 4 ‘Aprobarbital 342 22 357 39 28 arbital on 063 308 258 22 Benactyzine - - 382 - - Brallobarital 3.09 1 an 236 3 Butalbital 67 248 394 aa 34 Butetamate - - 390 - - Butbarbital 543 342 386 ass a2 Carbamazepine ~ - a8 368 - Clonazepam - - 465 403 46 Cycobarical 525 261 384 382 32 Cyelopentobarial 6 34 391 382 - Enalhlopymal 86s. 696 - 398 - Ethosuximide - - 301 276 23 Flavorate - - - - - Heptabarb 90 493 416 arr 39 Hevethal 3428 2039 - 451 - Hesebarbital 737 567 9 2a 43 ‘bomal 401 258 379 382 - \dobutal a2 477 - 387 - Mebeverine - - 448 - a Mephenytcin - - - 366 a7 Mesuximige - - - 387 48 Metharbial 269 199 a5 328 - Batbtal an oss - - - Methyiphenobartital 7.27 334 435 395 46 Nealbarbial 1022 619 47 ae - Papaverine - - 363 295 - Pentobarbtal 1096 807 428 383 aa Phenacemide - - 339 266 - Phenobarbital 3.09 13 379 235 a Phenyoin - - 431 381 a7 Primidone - - an 228 24 Secbutabarbital 49 33 a77 aa - Secobarbital 1628 nar a7 407 47 Sutiame - - 2s 27s - Tabutal 72 a7 403 370 - Thiam - - 56 476 - Thiopental - - 485 43 69 Vinbaritl 403 232 379 363 - Vial : : a4 : 4 Antidepressants © Column: ODS Hypersil (160 x 5mm id, Spm) The general screening systems, previously described, may be used oF systems HF and HAZ below. ‘System HE Gill, unpublished data after Kabea PM et al. (1981). Clin Chim Acta Mie 125-132, 1 Mobile phase: Acctontrle-phosphate butfer (pH 3.0; 30:70). To prepare the phosphate buffer, add 046ml nonylamine to. 1L 601 moll. sodium dihydrogenphosphate (1.19983/L) and adjust the pH to 40 by the addition of phosphoric acid. ‘System HAZ (Chiba K era. (1995). J Chromatogr B 668: 77-84 744 High Performance Liquid Chromatography ee . ke w@ 9 Ok ce ke ae pipramel 22 183 377 340 a9 142 - - Recommended HPLC systems 745 ca Paroxetine 226 337 56 153 vm Phenaine 1 - 184 - - - - - Protpyine a 36 aa 362 - - - - Removpide - - a4 - 3 - 88 - me-83) - - 316 - - - - - mvc¥-001) - - 368 - - - - - M(Ncw-008) - - an - - - - - Servalne - - 460 - 82 - 14s - (desmetyceratine) - - - - 70 - - - Tofenacia w - - - 53 - - - Trsodone 06 - 378 30s 33 127 - - “imipramine a7 ea 454 34s 83 159 185 - Minor) 18 - - - - - - - iasine - a7 22 23 - n - - Timeline a2 067 - 270 - - - - Minor) 29 - - - - - - - Antihistamines ‘Antimalarials The general screening systems, previously described, may be used. "The general screening systems, previously described, may be use, SS HA x HY wz HAA Wax HAY % a Rl [a a er fa “meme 3 220 ss - - 145 7 Antaalne 18 382 294 - - - - Astemiole - - 286 39 132 - - (ectemaol) 382 - - - - - (000 - 361 - - - - - Bromazine 27 aaa - - - - - Brompheniamine 4.1 - 267 - 139 - - Buclane 07 - 454 - - - - Garinormine 47 359 - - ne - - caine - - - 36 157 889 529 Choreciane 23 - 340 - - - - Chowphenamine 39 256 264 as 129 wos sa Cinnariine oa 60 - n 193 - - Clmastine 37 sot - 4 - - - Clemacle 48 420 - - - - - Gycline 29 40s - 48 - m4 se Noryelaine 22 - - - - - - Cyproheptadine 32 - as4 6s 1s - - Deptopine s an - 103 - - - Dimetindene sa 238 298 - - - - Diphenhydramine 3.3 393 336 - - 122 6 Diphenyipyraline 33 401 - - - - - Donamine aa - 259 - ma - - Hyéronaine 1 a7 326 s7 183 na 63 Isethipend a8 390 - - nas - - loatadine - 523 362 146 ns 109 133 ‘witinaed 746 High Performance Liquid Chromatography aK HY HZ HAA aX HAY * RI ® co ar ar aT Mebhydroin 3 atv = 53 Meclazine o7 se7 398 - 20 - - Mepyamine 39 8 2s7 - - - - Methapysene 41 3a 17 - - - - Methdiaine 6 - - - - 152 67 Phenindamine 25 397 - - - - - Pheniramine 4 283 206 - - 9s 4s Phenytoloamine 3.1 415 - - - - - Psotiten a4 435 - 6s 152 - - Promethazine 5 409 324 57 145 132 oa Propiomaine 2a 440 359 - - a ma Pyrobutamine 28 477 - - - - - Trenydiamine 4 317 - - - - - Thiasinamium - - - oa - - - reticulate Trimethobenzamide 47 27 - - - - - Tipelennamine 36 336 265 - - - - Tipline 32, 388 270 - 134 - - HA aK HY HZ HAA AX HAY ‘ @ RI a ca Chloroquine 152 732 246 2H so 127 36 Ginchenidine 31 306 214 - - - Ginchenine - 308 209 - 102 - - Halofantine - 200 - - 2 - - Hydrexychloroquine - 280 - 19 - 96 a2 Primaguine 14 - 276 - - - - Proguani - 379 - 38 136 - - Pyrimethamine 1 - 289 - ps - - Quinine 24 327 246 26 na a3 4s Antineoplastics: HA Hx HY HAA Rr AT Dextrorphan - 325 - - Anus The general scrcening systems, previously described, may be used, The general screening systems, previously described, may be used oF systems HAB and HAC below. Recommended HPLC systems 747 ‘System HAB Sparidans RW eal. (2000). J Chromatogr B Biomed Sei Appl 742: 185-192. |= Column: Cyy Symmetry (100 x 4.6mm id, 3.5 um) wit yy precolumn (20 x 3.8mm, 5 jm). Mobile phase: Acetonitrle-sodium phosphate buffer (25 mmol/L pH 6.8) (40:60). low rate: 1.3 mimi, Detection: Fluorescence (Hyg = 270.1, oy = 340.) (Note: Sin after each injection, fash column for 5 min at 1.5 mL min with acetonitrie-water (30:70). Equilbrate for about 8 min ‘ith the original eluent before injecting the next sample. ‘System HAC ‘Aymard G et al. (2000). J Chromatogr B Biomed Sci Appl 744: 27-240, Symmetry 1 Column: Cyg Symmetry (250 x 4.6mm i, Sym) with Cys precl- uma (Guard-Pak, uBondapak), Colum temperature: 37°C. Mobile phase: (A:B) Disodium hydrogenphosphate (0.04 mol/L) ‘with 496 (vv) octane sulfonic acid (0.25 mol/L)-acetontril. Aseratic elution: (50:50). low rate: 13 mLimin Detection: DAD (}.=261 nm between time 0 and 9min; k= 241 am ‘between time 9 and 20/min; — 254:nm between time 20 and end of the run (32 min), HAB HAC ca Ci ‘Rbacawr T ‘Amprenavie. 4 2s Efren - as Inginavie 42. 2 Benzodiazepines ‘System HI Gill, unpublished data |= Column: ODS Hypersil (200 x 3mm id. Spm) = Mobile phase: Methanol-water-phosphate buffer (58:25:20). To prepare’ the phosphate buffer, dissolve 11.038 g (0.092 mol/L) sodium dihydrogenphosphate and 1.136 (0.008 mol/L} disodium Inydrogenphosphate in suficient water to produce IL ‘System Hy Gill, unpublished data, 1 Column: As for System HI, above "© Mobile phase: Methanol-water-phosphatebutfer (asin System Hl) (70:10:20). ‘System HK Gill, unpublished data, afer RJ Flanagan et al. (1980). J Chromatogr 187: 391-398, 15 Column: Silica Spherisorb (250 x 5 mm id, 5 um). |= Mobile phase: Methanol to which has been added 100 pL perchloric acid pet lite. Cannabir ‘System HL Baker PB tal (1980) J Anal Toxicol 4: 145-1 "© Column: ODS Spherisorb (250 x 4.6mm id, 5 tm) ids ‘= Mobile phase? O01 mol/L. selfuric ackd-methanol-acetonitrile (7:8:9) can System HL “Cannabiehromene 79.08 Cannabicytl 1478 Cannabidel 7a7 Cannabidole acid 876 annabigerol aig annabinal ng Cannabivacin 747 -¥Tetrahydrocannabino! 1407 _Tetrahydrocannabino! 1335 Tetrayérocannabinalc acid 2583 Tetrahydrocannabivaric acid 1464 Tetrahydrocannabivarin arg Cardiac glycosides ‘System HM ‘Cobb PH (1976). Analyst (Lond) 101: 768-776. "© Column: Silica LiChrosorb $160 (250 x 4mm id, 10pm), 1 Mobile phase: Cyclohexane-ethanol-acetic acid (60:91), ‘System HM © Digtowgenin| 20 Digitoxigeninbisdigtoxosde 39 Digitoxigenin monodigitoxoside 28 Digitoxin 54 Digosgenin 45 Digongeninbscigtoweide a2 Digosigenin monodigitoxoside 55 Digoxin na Gitaloxin 68. Gioxigenin a7 Gitoxigenin bietigtnoside 6s. Gitxigenin monedigtoxoide 45 Gitoxin 86 Lanatosde A wa Lanatosde & a8 395. Lanatosde C HL a HK HK HY Hz HAA HAX HAY. « % xe ® @ ar aT, ar ar "Rcecarbromal = = ss 429 374 Alprazolam - - 279 - - - - - . Bromazepam - - 209 - - - - - 748 High Performance Liquid Chromatography a cg x HY HZ HAA HAXOHAY. K k Cj Rr I aT co ar aT Bromizoal = 365 307 29 = Bratzolam - - - 404 - 46 - 74 79 Carbromal - - - a0 a7 39 - - - Chleriazepoxide - - 297 - - - - - - Clbazam - - 003 - - - - - - Clomethiazole - - - 295 22 - 16 - - Clonazepam - - 03s - - - - - - Clorazepic acid - - 200 - - - - - - Demoxepam - - 003 - - - - - - Diazepam - - 249 - - - - - - Flumazenl - - - 387 aur 26 - - - Flunitrazepam 315 - 047 3 305 56 186 - - Flurazepam - 319 6s 397 305 42 - 10s ss lutetimie - - - 426 401 48 - 66 62 Ketazlam - - 0.04 - - - - - - Loprazolam - - - 388 - - 134 - - Lorazepam - - o14 - - - - - - Lormetazepam 632 - 0.08 387 463 62 - - - Medazepam - - 444 - - - - - - Methaqualone - - - 459 400 54 - 6a 74 Methypoyon - - - 37 302 - - - - Midazolam 975 2a 59 399 306 42. 149 102 63 Nivazepam 296 - 149 448 370 42 169 63 6 Nordazepam - - 19 - - - - - - Orazepam 42 - 073 - - - - - - Prazepam - - 219 - - - - - - Quzzepam - - - - 766 375. - ng 7 TTemazepam 568 - os an 438 55 186 a9 67 ‘xazepam - - ova - - - - - - ‘Viazolam 438 - 183 476 390 42 14 oa 67 Not detected - - - - - - - - - Zolpidem - - - - 291 32 ng - - Zopiclone : : : 331 269 23 - 7s 38 Cardioactive drugs The general scrcening systems, previously described, may be used ‘Aimalne Auzosin Amiodarone Monadesethy Amiodarone Apvindine Bamethan Benathiazide Betahictne Breyium tosiate HA x ze 24 18 09 a 43 aK ® a3 43 250 ay ® 27 476 415 275 WZ ar ‘ale ST WA HK HY HZ «HAA a “Bphening SOO captopril 31628321 Glazapei 200 45044 Clazapniate - - we ligne 120025819828 Clopamide a7 HO - Debrisoquine 2m ms - Ditiazem - a 4S Deacety - - - - assem Desmethy - - - - ‘itazem Recommended HPLC systems 749 ‘Cardioactive drugs, continue HAA HAWK HY HZ ~ aT Desai — ss Disopyramide 24 M5] na WMonadesio- 18 = - - Propylccopyramide Enalapril - 2 - 1s a4 Eneainide - 33 - Felodiine - 60-82 Fecsinide - #9052 Hyeralzine - 13001219 Isoxsupine os 383 amt - Label! 17365-2903 - Lidofizine os 30 - Lisinopril - as Loresinide le 45 so Methyidopa - so 8 Mesietine 1200 3290 ns Minos! - a 24 98 Natt - - 409 158 Nitedipine 02 52746472195 Pargvline 02 - 2 - Pentaerthriy - oa - (pentaeriteyd) —~ - - 231 Pentosifline - 355 22S. Petindopi - - - 1137 (petindopriat) = aa - Phenosybenzamine 0.1 396 = = - Phentolamine 17368 ae Pramalium 2 340 - rare Prazosin os sn 25106 Procsinamide ee ee en N-Acetylro 3 - - 1s cainamide Quinapi - - - 54168 Quinidine 21 32S 26 Ramipi - - - 420187 Rescinnamine os 496407 - Reserpine - 47st 164 Sala 2 26 2 38 Tocsiide 12007 Ra Talaaline 210s - Trandolapi - - - so Trandolapriat - - - a Tiimetasidine ae - 6 Verapamil 26447867 154 Minor) we : 6s Diuretics ‘System HN Rill eal, unpublished data, after Tisdall PA era. (1980). Clin Chem 26: 702-706. © Column: ODS Hypersil (160 x 5mm id, Sym) ‘= Mobile phase: Acctontrile-water containing 10mL/L acetic acid (30:70), HN wx HY HAA « a Teetsaamige a a6 63 Amilride - 2719036 Bendrofumethiasie 15.35 soe 186 Benzthiaside 932 - as Clorohiside oss - 20 Chloralidone 128 36708 Clopamide 401 a7 mo - orexolone 726 - an Cycopentianide 16.45 - 4300 Cycothiasde 1078,1191, = 43 and 12.81 racic acid - so 497 Furoeemide - 250 30 152 Hydrechlorathianide 07 2a 5 Mefrside 267 - 7 Methycothande 382 - aes 154 Metolizone 429 - an Spironolactone - sm 539207 Teamterene - 20a 26387 ‘Ticlormethiasde aa - a 149 Xipamide - a8 138. Drugs of abuse ‘A comprehensive HPLC method for the screening of common drugs of| use fs described in Chapter 1, Table 124. Furthermore, an additional ight systems (HBC, HBD, HBE, HBE, HBG, HBI and HB}) are provided in Chapter 11, Table 11. WA HC OBX HY HZ HAR ~~ * 7 7 * ® Sheng Amfetamine «09098248 a Bensftamine = 12, 1S Benzoylecgenine 09 - = - 238-1797. Bufotenine Bo Cannabiiol ~ = 990 902 Cannabinal ne Cocaine 28 - MB 2893319 sec Se Diamorhine 3.066 340282 Diethytypt ee Dimethyitypt> = = B= om - an ketamine - = 222496 lsewicad = 08 8 Lyserside Ce ‘panied 750 High Performance Liquid Chromatography Local anaes HY SE SHAR The gencral screening systems, previously described may be used, as well Hem HO or Ht low Mescaline 13217272243 ‘System HQ Meanfeume 2 207 222 216 248g CHR tal (RD, Jaman 1 8516 Matadors | 22 M03 4038S TSB itp Methane lev soitn of phoxporc acid Metnlenediog- —- 098 266248218 Ihexylamine (30:70: 100: 1.4), Mepuepedonr, © 27252 2281 TT tJ roma 30: 185-163 Monee 3608 == 73 Calum: As for System H above rome 1 Notephs: Metra 1% tion of phosphoric acide Mopine 3813-200, 82.833 amine (100-100:14, NMving = fe Psion a eee Psilacybine - oe - ves - kk K aR ORT Tenoane 07 2006 Talon 358 a3 Ergot alkaloids Dipiacine «09719 «085 «366. «310.41 System HA, previously described, may beused or Sytem HEsbelow, —Huteine 12897 = 382 System HP Gi el, wap ds, after TwitcbeeB) ot al asry.¢ CUmwmmcaine S028 Crater iso-04 Column: ODS Hypersil (100 x 5 mm i, 5 jum). Cocaine 28 268 MB 28933 Mot pines Metnanl-popbate bur (60:40), To prepare the Setoveeene 09 S68 = phowphitc ute, dhe 348g (0022 mol) sodium diogens gone = Pophate and 003g (002m. daodiom hyrosenpomhate—cydomatyeane ST Ieasicn water to produce rere 5 fonite Sa Keamine 5 Gn aaa ce os 079 - 2885826 HA HP 1M (monoethy! Ww - - - - - i i renee = * = Mepracane 09109 == «296260 268 Dihydroergocristine - 183 Methohextal - . - 503 484 Divaeecntne : iso Onbupecine 1625085 sas Powreane 45ST Dinvereergosamine os nm Pramocaine 06 - 2480 4150 ~ 6S Exsocorning of 102 Prilocaine 1 1380 - - - 27 erocistne 03 va Ergocryptine 04 152 Procaine 1 - e425 Ergometrine 4 0s0 Propofol 5 7 - - 7 se ceomes ° G2 ommeacang 27138 2 Eaosnne ° we Qiwonie = «22-2 cee a 77, Tecan 2 1625133894 bose ae - oss soepze 26 00 Lysergamide os 033 Narcotic analgesics pape se 08 00 Sytem HA oF HC, previouly dex, maybe wed o Sytem HS, Usage so methypepymise - 18 below Unepe o7 183 Sytem Hs ye nu ss —_BakerPB, Gough TA (1981. J Chromatogr Si 19:485-49 Methegometine oa 083m Cs: Aminopropy-bnet sia Spherion SNH (250 x mm Methysergide 04 233 id. Sum). ene ° 23 Nsbie ps: _Acctontsecerabuslammoniom phosphate, (0.005 mol/L, pH 75 (85:15). Recommended HPLC systems 751 HA HC HS. we ay HZ HAA AX HAY K k Cj Rr I ar eT ar aT ‘Alphaprodine 28 - - 363 737 Beztramice 02 - - sos - 225 - - - Buprenorphine 04 0.05 - 397 339 5 4 - - Codeine 48 121 19 266 237 19 5 or a4 Morphine 38 3 5.16 - - - - - - M (nor?) 31 351 - - - - - - - cyeazacine 2a - - - 289 - - - - Dextomaramide o7 009 - 440 390 - 18 - - Dextropropoxyphene 19 019 - - 374 76 158 - - Norpropoxyphene 13 - - - - - - - - Diamorphine 3 oss: 035, 340 2a - - 79 aa G-Monoacevimorphine 36 os 1 - - - - - - Morphine 38 3 5.16 - - - - - - Dinyarocodsine 72 25 - 261 208 2 47 - - Dihydromorphine 57 275 - 237 156 - - - - Dipipanone 22 161 - 500 363 - - - - Ethoheptazine 33 155 - 350 - - - - - Ethyimarphine 37 106 15: 291 Dae - - 67 36 Fentanyl os um - 373 299 - 142 na 6 Hydromorphone 79 - - 240 187 - - 58 34 Ketobemidone 28 - - 298 265 - - - - Levalorphan 19 146 - 386 2a - - - - Levorphanol 44 32 - - 265 - - - - Meptaznol 31 - - - 269 - - - - Methadone 22 103 - 440 343 as 158 sas MeDoP) 28 - - - - - - - - MeeMoP) 02 - - - - - - - - Morphine 38 130 516 200 182 18 33 5632 Morphine - 156 - - - - - - - Srglucuronide Novide 32 - - - - - - - - Nalorphine 1 029 - 260 2a7 - 48 - - Nalosone 14 oa7 - - 238 2 4 - - Norcodeine a4 351 - - 238 - - - - Normethadone - 053 - - 366 - - - - Noxmorphine 29 392 - - 1a - - - - Npipanone - 035 - 466 - - - - - Oxycodone 69 os - 27 246 - - os sa rymorphone 67 - - - - - - - - Oxymorphone o - - 27 18 - - - - Pentazocine 18 os7 - an 288 a8 vs 99 ss Pathisine 28 oss. - 245 281 a2 ns 92 48. M (nor?) wv 208 - - - - - - - Pethidinie acd 28 - - - - - - - - Phenazocine 1a 03 - 409 299 - - - - Phenoperidine os 01 - a4 - - - - - Nowpethidine 7 204 - - - - - - - Pathisine 28 oss. - - - - - - - Pictramide 06 01 - a7 343 - - - - Thebacon ay as - a3 - - - - - Tramadal - - - 228 267 29 - - - 752 High Performance Liquid Chromatography Oral hypoglyacemics and antidiabetics The general screening systems, previously described, may be used ee) Tarbutamide Chlerpropamide Gibenclaige Glctazice Gipixice Metformin Tolazamide Talbutamide wx Rr 450 6x7 536 478 oo 482 477 wy a ar 411 ang a3 sm 483 423 as 224 HZ ar 5 144 a8 45 vw 6a 59 Pesticides ‘System HAO (Osseton MD, Snelling RD (1986). J Chromatogr 368: 265-271 © Column: ODS Hypersil (160 5mm id. Spm), stainless see. Mobile phase: Acetonitie-water (60:40). low rate: 2mL/min, 1 Detection: DAD (200-450.nm). ‘System HAP (Osseton MD, Snelling RD (1986). J Chromatogr 368 265-271 1 Column: Silica Spherisorb SSW (280 x 5mm id.) 1 Mobile phase: Dichloromethane-isoctane (60:40), low rate: 2mL/min, Detection: DAD (200-450.nm). For more information on screening pesticides, see Chapter 16, Table 161 Phenothiazines and other tranquillisers The general screening systems, previously described, may be use HZ WAR HAX HAY HAZ K RL a ar ar ar ar k ‘Reepromazne aT 350 = TE = ‘aacyclono! 2 - - - - a7 45 - Benzoctamine Ww 380 322 - - - - - Butaperazine 34 464 406 - - - - - Captodiame - 61 - - 202 - - - (Cloriazepoxide - 363 285 32 152 69 53 168 CChlormezanone - - 234 - 15 6 53 - Chlorpromazine a 456 350 a 6 v7 BASE 2068 M (nor) 22 - - - - - - - (sulfoxide) - - - - - a4 43 062 CChorprothisene 3 459 353 101 - 176 83 - Clopenthiao! - 438 an - - - - - Clorazepic acid - 475 388 56 - - - - Corazepate - - - - 184 - - - Fuanizone - 43 349 - - - - - Flupenticl 12 475 435 107 wa 137 7s - Sutlorde 13 - - - - - - - Fluphenazine 2 462 an 101 wa 136 72 - Fuspirlene - 538 - - - 183 98 - Haloperido! 2 a1 316 58 144 mm 62 072 Levomepromazine 32 435 381 75 - 152 72 182 Loxapine u 407 336 - 146 - - - Mesordazine 5 - 237 a4 - 101 5 - Onpentne 07 402 - - - - - - Pecazine a9 443 382 - - 153 7 - Penfluridot - 659 656 a4 202 - - - Peratine - 403 am 63 - - - - Pesicyazine 3 a0 356 44 - 102 sa - Perphenazine 19 228 395 72 16 1a 63 328 Pimeride o7 508 - ng 172 - - - Pipamperone - 299 2 27 109 - - - Piptiarine - 431 - - 147 - - - Prochlorpeazine 30 450 223 10.4 - - - - Promazine 59 407 226 59 - - - - Recommended HPLC systems 753 HA aK HY HZ WAR HAX HAY HAZ © RI @ a ca ar ar % Prothipendyl a4 7388 = Suloiazine - 421 - 48 - - - - sulpiride - 259 235 2 39 - - 02 Thiopropanate 1 483 - - - - - - Thioproperazine al a7 305 154 152 - - - Trieriazine 52 490 407 135. 72 - oa 388 Mesorgazine 5 - - - - - - - Totvene 38. aan ams os. - - - - Tetlupomazine 27 484 454 3 - 173 89. - Steroids 1 Flow rate: 15 mimi, System HATa 1 Detection: UV (3.=240, 210 and 280 nm), Walters Mj etal (1990). J Assoc Of Anal Chem 73: 904-926 ‘System HAR © Column: ODS Zorbax (250 x 46mm id, Spm), stainless stl, Lune Leta. (1994). J Forensic Sei 39: 74-8. 1 Eluent (A) Methanol 5 Columns ODS Zorbax (250 x 4.620 i, 5pm) 1 sort euton: (100) 1 Molle phase (A) Water-methano. 1 Hw rate: 13 mLimin 1 Gradient elution: (30:70) to (0 100) ver 15 xin with 15min bold 1 Detection: UV (i= 240, 210 and 280 nm). 1 Flow rates LO mL/min System HAT Detection: DAD. Walters Me al (1990). J Assoc Off Anal Chem 75: 904-926, System HT 4 Clunn: ODS Zorba (250 x46mm id, pm), sainks see, ROS 10, Fasko W) (1979). J Chromatogr Biomed Appl 162 273-28 1 Hluents(A:8) Methanl-vater. 1 Columns Silica Zorba SI. (250 x 4.620 iy 5m) 1 eortic elution: (75:25) 1 Mobile phase: Methylene choride-mcthanol (97:3). SS HT ax “ wz HAA HAR HATa ‘HATS % @ @ er a BRT RT «ORT Bacometasone a aa ~ ~ - ~ ~ ~ Diproponate - - m - - - - - Betamethacone - - - 142 13a - - - Setamethatone valerate - - se - - - - - Bodenone - - - - - 074 - 076 Undecylenate - - - - - - 198 Conizone 24 - 372 - - - - - Dexamethasone a8 - 381 34 aaa - - - Fluosymesterone - - a7 - - ove - oz Hysrocrizone se 40a 349 - ww - - - Hyeronprogesterone - nose - - - - - Metenoione - - - - - - - - estate - - - - - - 126 ass Enantte - - - - - - 187 - Methandienone - - - - - 086 - os7 Methandsl - - - - - 12s - 129 Dipreponate - - - - - - - 275 Methyoredniolone 75 426 390 - 189 - - - Methyestortrone - - 587 - - a7 - aa Nandone - - - - - oa - os2 Notethistrone - 536 os - 24 - - - Preciolone 84 401 361 as 14 - - - Prednisone 34 250 340 26 142 - - - Progesterone - on 28 - ns - - - ‘pitied 754 High Performance Liquid Chromatography — a: Ssfonamider Preninesomuane mem nom om mom Cobb PH, Hill G Column: Sitica Spherisor’ (250 x4 mm id, 5 jm). 1 Mobile phase: Cyclohexane-ethanol-acetic acid (85.7:11.4:2.), (1976). J Chromatogr 123: 444-447 HU K Prihadvsuatharole 140 Succinylsutatiazole 168 Sulfadoxine 44 Sulfamerazine 81 Sulfaguinoaline 48 Sutfacetamide 7 Sulfachorpyridazine 33 sutadasine 87 sufadimidine ay Sufafurazle 60 Sufamethoxazole 48 Sufamethonydazine 82 Sufamethonypyidasine 7s Sufamoxole 126 sulfatide 89 Sulapyridine 38 sulathigole B4 Xanthine stimulants The general scrcening systems, previously described, may be used * faa “Gene 0230s) Diprophyline - ws or Fenetyline - 3607 - Pronphyline or 3 - - ‘Theebromine ol 2621838 Treophyine or 26a Additional systems ‘System HAD “Aymard et al. (2000). J Chromatoge Biomed Sci Appl 744: 22: Colum: Cyg Symmetry Shield (250 x 4.6 mm id, 5 um) protected bby 2)im Upchurch filter. = Column temperature: 30°C. 1 Mobile phase: (A:B) M/15 potassium dihydrogenphosphate with 1% (v) octane sulfonic acid: acetonitrile. Mobile phase (MP) 1 (95:5) atflow rate I mL/min; MP 2: (80:20) at flow rate I m/min; MP (0:70) at flow rate 12:mL/min, 1 Elven switching programme: At injection, MP1 tothe column. Prom time 12 min to 30min, MP2 tothe columa, From time 30 min, MP3 to the column to rinse it From time 35 min to 40min, equilibration with MPL 1 Detection: DAD (2= 260m) k Compound Wine a2 Didanosine 38. Stavudine 66 Zidovudine ar ‘acavie mi Neviapine Recommended HPLC systems 755 ‘System HAF Tanaka E et al. (1996). J Chromatogr B Biomed Sei Appl 682: 173-178, Columns ODS TSK-gel Super (100 4.6mm i, 2 um). Mobile phase: (A:B) Acctonitsile-5 mmol/L sodium dihydrogen: phosphate (pH 6). § socratie elution: (48:55), 1 Flow rate: 0.65 mL/min 1 Detection UV (i, =254 nm). ‘System HBB Taninaka C et al. (2000) J Chromatogr B Biomed Sci Appl 738: 405-411 Colom: Cyy (250 x 6.0mm i, 5 um) Eluent: (AB) Acetontrile-30 mmol/L phosphate buffer (pH 7.2) Isoerati elution: (43:57) Flow rate: 1.7 mL/min, Detection: Electrochemical (working electrode: glasy carbon; refer. cence electrode: AgiAgC). Retention time (ia) Compound Retention time (in) Compound 53 Clnazepam 68 Clrthromin 66 Bromazepam 68 Eryvomycin on Niazeram 96 Aathromycin 137 Triazolam 163 Reoxithromycin 150 Lorazepam TT 184 Eola system HAE 210 Chlrdiareponide Proust Vet al. (2000). J Chromatogr B Biomed Sei Appl 742: 453-458 208 Diazepam 1 Column: Cyy (Lichrospher, 100 RP-18, Spm) with Cyy precolumn 322 Futazolam (Cichrospher RP-18, Sum) 1 Mobile phase: (A:B) Acctontrle-25 mmol/L. sodium phosphate modified with dithylamine (0.9%) and tetahydrofuran (1%), pH ‘System HAV. 30. Rutledge DR et al. (1994). J Pharm Biomed Anal 12: 138-140. © Colunm: RP-short alkyl chain, silanol-deactivated (SCD 100; 250 x 4.6mm id), stainless see. 1 Mobile phase: (A: 1) Methanol-0.04 mol/L dibasic potasium phos phate (pH 5.3). 5 socatic elution: (50:50) s Flow rate: | mein, © Detection: UV (=237 nm). k Compound 2 Celproit 23 Propranoel 36 Diltiazem deacetylitizem 51 Diltiazem desmethyditiazem 61 Ditiaem 64 Imipramine 82 Verapamil ‘System HBA Sastre“Toraf J, Guchelaar H-} (1998). J Chromatogr B Biomed Sci Appl 720: 89-97 Column: Cy base-deactvated silica (125 » 4.6mm id, 5 um) wi base-deactvated Cig precolumn (20 x 4.6mm id, 5 um). ws xcrati elution: (44.8:552) Flow rate: 0.5 mL/min. = Detection: UV (= 260m). Retention time (min) Compound avin 70 Saquinavir 20 Netinavie 94 Amprenavir 222 Ritonavir 286 Efavirenz ‘System HAK Le Guellee Cet al (1988). J Chromatogr Sei Appl 719: 227-238. 1 Colton: Cyg Symmetry (280 x 4.6mm il, 5 um) with Cy precol- uma Symmetry sentry = Mobile’ phase: (A:B) hydrogenphosphate 5 Elution programme: (50:50) to (70:30) in 15 xi, 2 Flow rate: mein, © Detection: UV (= 313 nm). Acetonitrile 20 mmol/L potassium di: 1 Eluene: (A'B) Acetonitrle-50 mmol/L potas dihydeogen- RAtGREgn Wine Ci) Compound phosphate (pH 7.5, containing 500 triethylamine. a trp 1 sora elution: (60:40). ee a Flow rate: 2mlJin 62 Clonazepa 1 Detection: Fluorescence (hy = 255 yg = 3152). 76 Nordazpam 93 Clbazamm Nor detected Phenobarial ‘Retention tie (min) Sap Not detected Phenytoin 38 Ethromycin 157 Clarithromycin ve ‘System HAL va Rosthromyein Boukhabea A eal (1990). J Chromatogr 529: 210-26. 207 Athromycin Colum: Cy Novapak (150 x 4.6mm id 5 ym).

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