duoc dien vn iii 6797 2

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Dược đin Vit Nam III 1-ACID ACETYLSALICYLIC Acidum acetylsalicylicum Aspirin C9H8O4 P.t.l: 180,2 Acid acetylsalicylic là acid 2-acetoxybenzoic, phi cha t99,5 đến l01,0% C9H8O4, tính theo chế phm đã làm khô. Tính cht Tinh thkhông màu hoc bt kết tinh trng, không mùi hoc gn như không mùi. Khó tan trong nước, dtan trong ethanol 96%, tan trong ether và cloroform. Chy khong 143oC (Phlc 5. 19, Phương pháp 3). Định tính Có thchn mt trong hai nhóm định tính sau: Nhóm I: A, B Nhóm II: B, C, D A. Phhng ngoi (Phlc 3.2) ca chế phm phi phù hp vi phhng ngoi ca acid acetylsalicylic chun. B. Đun sôi 0,2 g chế phm vi 4 ml dung dch natri hydroxyd loãng (TT) trong 3 phút, để ngui và thêm 5 ml dung dch acid sulfuric l0% (TT). Ta kết tinh được to thành. Ta sau khi được lc, ra vi nước và sy khô l00 - l05oC, có đim chy t156 đến 161oC (Phlc 5.19). C. Trong mt ng nghim, trn 0,1 g chế phm vi 0,5 g calci hydroxyd (TT).

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  • Dc in Vit Nam III

    1-ACID ACETYLSALICYLIC

    Acidum acetylsalicylicum

    Aspirin

    C9H8O4 P.t.l: 180,2

    Acid acetylsalicylic l acid 2-acetoxybenzoic, phi cha t 99,5 n l01,0%

    C9H8O4, tnh theo ch phm lm kh.

    Tnh cht

    Tinh th khng mu hoc bt kt tinh trng, khng mi hoc gn nh

    khng mi. Kh tan trong nc, d tan trong ethanol 96%, tan trong ether v

    cloroform.

    Chy khong 143oC (Ph lc 5. 19, Phng php 3).

    nh tnh

    C th chn mt trong hai nhm nh tnh sau:

    Nhm I: A, B

    Nhm II: B, C, D

    A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng

    ngoi ca acid acetylsalicylic chun.

    B. un si 0,2 g ch phm vi 4 ml dung dch natri hydroxyd long (TT)

    trong 3 pht, ngui v thm 5 ml dung dch acid sulfuric l0% (TT). Ta kt tinh

    c to thnh. Ta sau khi c lc, ra vi nc v sy kh l00 - l05oC, c

    im chy t 156 n 161oC (Ph lc 5.19).

    C. Trong mt ng nghim, trn 0,1 g ch phm vi 0,5 g calci hydroxyd

    (TT).

  • un hn hp v cho khi sinh ra tip xc vi ming giy lc tm 0,05 ml

    dung dch nitrobenzaldehyd (TT) s xut hin mu xanh l cy hi vng, hoc

    xanh l cy hi xanh lam. Lm m t giy lc vi dung dch acid hydrocloric

    long (TT), mu s chuyn thnh xanh lam.

    D. Ha tan bng cch un nng khong 20 mg ta thu c t php th B

    trong l0 ml nc v lm ngui. Dung dch thu c cho phn ng ca salicylat

    (Ph lc 7.l).

    trong v mu sc ca dung dch

    Ha tan l,0 g ch phm trong 9 ml ethanol 96% (TT). Dung dch phi trong

    (Ph lc 5.12) v khng mu (Ph lc 5.17, phng php 2).

    Tp cht lin quan

    Trong bnh nh mc dung tch l00 ml, ha tan 0,15 g ch phm trong l0 ml

    dung dch tetrabutylamoni hydroxyd 0,1 M trong 2 - propanol, yn 10 pht.

    Thm 8,0 ml dung dch acid hydrocloric 0,1 N v 20,0 ml natri tetraborat l,9% v

    trn u. Thm 2,0 ml dung dch aminopyrazolon l,0% v 2,0 ml dung dch kali

    fericyanid l,0%, trong qu trnh thm cc dung dch ny lc lin tc. Sau 2 pht,

    pha long n 100,0 ml bng nc. yn 20 pht. o hp th ca dung dch

    bc sng 505 nm trong cc o dy 2 cm, dng nc lm mu trng. hp th

    thu c khng c ln hn 0,25 (khong 0,l% biu th bng acid

    acetylsalicylic).

    Acid salicylic

    Khng c qu 0,05%.

    Ha tan 0,l0 g ch phm trong 5 ml ethanol 96% (TT), thm ngay 15 ml

    nc c lm lnh trong nc v 0,05 ml dung dch st (III) clorid 0,5%.

    Sau 1pht dung dch ny khng c c mu thm hn mu ca dung dch i

    chiu chun b ng thi bng cch cho hn hp gm 0,05 ml dung dch st (III)

  • clorid 0,5%, 0,1 ml acid acetic (TT), 4 ml ethanol 96% (TT) v 15 ml nc vo 1

    ml dung dch ca 5,0 mg acid salicylic trong 100 ml ethanol 96% (TT).

    Clorid

    Khng c qu 0,015% (Ph lc 7.4.5)

    Dung dch S: un si 4,0 g ch phm vi l00 ml nc trong 5 pht,

    ngui, thm nc va 100 ml v lc.

    Ly 8,3 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.

    Sulfat

    Khng c qu 0,040% (Ph lc 7.4.12).

    Ly 9,4 ml dung dch S, pha long vi nc va 15 ml v tin hnh th.

    Kim loi nng

    Khng c qu 20 phn triu (Ph lc 7.4.7).

    Ha tan 0,75 g ch phm trong 9 ml aceton (TT) v pha long vi nc va

    15 ml. Ly 12 ml dung dch ny th theo phng php 2. Pha long dung dch

    ch mu l00 phn triu bng hn hp gm 9 th tch aceton (TT) v 6 th tch nc

    c dung dch ch mu 1 phn triu chun b mu i chiu.

    Mt khi lng do lm kh

    Khng c qu 0,5% (Ph lc 5.16).

    (l,00 g; p sut gim; phosphor pentoxyd).

    Tro sulfat

    Khng c qu 0,l% (Ph lc 7.7, phng php 2)

    Dng l,0 g ch phm.

    nh lng

  • Ha tan 1,000 g ch phm trong 10 ml ethanol 96% (TT) trong bnh nn

    nt mi. Thm 50,0 ml dung dch natri hydroxyd 0,5 M. y nt bnh v yn

    trong 1 gi. Chun bng dung dch acid hydrocloric 0,5 M, dng 0,2 ml dung

    dch phenolphtalein (CT) lm ch th.

    Song song lm mu trng.

    1 ml dung dch natri hydroxyd 0,5 M tng ng vi 45,04 mg C9H8O4.

    Bo qun

    Ch phm c bo qun trong chai l nt kn, trnh nh sng.

    Cng dng

    H nhit, gim au, khng vim.

    Ch phm

    Vin nn aspirin.

    2 -ACID ASCORBIC

    Acidum ascorbicum

    Vitamin C, Acid L-ascorbic

    C6H8O6 P.t.l: 176,1

    Acid ascorbic l (R)-5-[(S)-1,2-dihydroxyethyl]-3,4-dihydroxy-5H-furan 2-

    on, phi cha t 99,0 n 100,5% C6H8O6.

    Tnh cht

    Tinh th khng mu hay bt kt tinh trng hoc gn nh trng, b bin mu

    khi tip xc vi khng kh, nh sng v m. Khng mi hoc gn nh khng mi.

    D tan trong nc, tan trong ethanol 96%, thc t khng tan trong cloroform v

    ether. Chy khong 1900C cng vi phn hu.

    nh tnh

  • C th chn mt trong hai nhm nh tnh sau:

    Nhm I: B,C

    Nhm II: A, C, D

    Dung dch S: Ha tan 1,0 g ch phm trong nc khng c carbon dioxyd

    (TT) v pha long n 20 ml bng cng dung mi.

    A. Ho tan 0,10 g ch phm trong nc v pha long ngay n 100,0 ml

    bng cng dung mi. Cho 1,0 ml dung dch mi pha vo 10 ml dung dch acid

    hydrocloric 0,1 N v pha long n 100,0 ml bng nc. o ph hp th t ngoi

    (Ph lc 3.1) ngay sau khi dung dch c pha long. Dung dch ch c duy nht

    mt cc i hp th 243 nm. Gi tr A(1%, 1 cm) 243 nm t 545 n 585.

    B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng

    ngoi ca acid ascorbic chun. Dp vin cha 1 mg ch phm.

    C. pH ca dung dch S nm trong khong 2,1 n 2,6 (Ph lc 5.9).

    D. Thm 0,2 ml dung dch acid nitric long (TT) v 0,2 ml dung dch bc

    nitrat 2% (TT) vo 1 ml dung dch S, s xut hin ta mu xm.

    trong v mu sc ca dung dch

    Dung dch S phi trong (Ph lc 5.12) v mu khng c m hn mu

    mu NV7 (Ph lc 5.17, phng php 2).

    Gc quay cc ring

    + 20,5 n + 21,5o (Ph lc 5.13)

    Ha tan 2,50 g ch phm trong nc v pha long n 25,0 ml bng cng

    dung mi tin hnh th.

    Acid oxalic

    Khng c qu 0,2%.

    Chun b ng thi dung dch th v dung dch i chiu nh sau:

  • Dung dch th: Ha tan 0,25 g ch phm trong 5 ml nc. Trung tnh ha

    bng dung dch natri hydroxyd 2 M vi giy qu (CT).

    Dung dch i chiu: Ha tan 70 mg acid oxalic trong nc v pha long

    n 500 ml bng cng dung mi, dng 5,0 ml dung dch ny chun b mu i

    chiu.

    Thm ng thi vo mi dung dch trn l ml dung dch acid acetic 2 M

    (TT) v 0,5 ml dung dch calci clorid 0,5 M (TT). yn trong 1 gi. Dung dch

    th khng c c hn dung dch i chiu.

    ng

    Khng c qu 5 phn triu.

    Xc nh bng phng php quang ph hp th nguyn t. (Ph lc 3.4,

    phng php 1).

    Dung dch th: Ha tan 2,0 g ch phm trong dung dch acid nitric 0,1 M

    va 25,0 ml.

    Dung dch chun: Chun b cc dung dch chun ng c cha 0,2; 0,4 v

    0,6 phn triu bng cch pha long dung dch ng mu 10 phn triu bng dung

    dch acid nitric 0,1 M.

    o hp th 324,8 nm, dng n cathod rng ng lm ngun bc x

    v ngn la khng kh- acetylen. Dng dung dch acid nitric 0,1 M hiu chnh

    my v zero.

    St

    Khng c qu 2 phn triu.

    Xc nh bng phng php quang ph hp th nguyn t. (Ph lc 3.4,

    phng php 1).

    Dung dch th: Ha tan 5,0 g ch phm trong dung dch acid nitric 0,1 M

    va 25,0 ml.

  • Dung dch chun: Chun b cc dung dch chun st c cha 0,2; 0,4 v 0,6

    phn triu bng cch pha long dung dch st mu 20 phn triu bng dung dch

    acid nitric 0,1 M.

    o hp th 248,3 nm, dng n cathod rng st lm ngun bc x v

    ngn la khng kh - acetylen. Dng dung dch acid nitric 0,1 M hiu chnh

    my v zero.

    Kim loi nng

    Khng c qu 10 phn triu (Ph lc 7.4.7).

    Ly 2,0 g ch phm th theo phng php 4. Dng 2 ml dung dch ch

    mu 10 phn triu chun b mu i chiu.

    Tro sulfat

    Khng c qu 0,l% (Ph lc 7.7, phng php 2).

    Dng 1,0 g ch phm.

    nh lng

    Ha tan 0,150 g ch phm trong mt hn hp gm 80 ml nc khng c

    carbon dioxyd (TT) v 10 ml dung dch acid sulfuric 1 M. Thm 1 ml dung dch

    h tinh bt (CT). Chun bng dung dch iod 0,1 N cho ti khi xut hin mu

    xanh tm bn vng.

    1 ml dung dch iod 0,1 N tng ng vi 8,81 mg C6H8O6.

    Bo qun

    Trong chai l kn, trnh m, trnh tip xc vi kim loi v nh sng.

    Cng dng

    Vitamin chng scorbus v l cht n nh dc phm (chng oxy ho).

    Dng tr liu thiu vitamin C.

  • Ch phm

    Vin nn, vin nang, thuc tim.

    3-ACID BENZOIC

    Acidum benzoicum

    C7H6O2 P.t.l: 122,1

    Acid benzoic l acid benzen carboxylic, phi cha t 99,0 n 100,5%

    C7H6O2, tnh theo ch phm lm kh.

    Tnh cht

    Tinh th hnh kim hay mnh khng mu hoc bt kt tinh trng, khng mi

    hoc thong mi cnh kin trng. Kh tan trong nc, tan trong nc si, d tan

    trong ethanol 96%, ether, cloroform v du bo.

    nh tnh

    A. Ho tan 1 g ch phm trong 8 ml dung dch natri hydroxyd 0,1 N v

    thm nc va 100 ml. Dung dch ny phi cho phn ng ca ion benzoat (Ph

    lc 7.1).

    B. im chy: 121 - 124oC (Ph lc 5.19).

    trong v mu sc ca dung dch

    Dung dch S: Ho tan 5,0 g ch phm trong ethanol 96% (TT) c

    100,0 ml.

  • Dung dch S phi trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng

    php 2).

    Cc hp cht cha clor

    Cho vo chn nung 0,50 g ch phm v 0,70 g calci carbonat (TT), trn u

    vi mt lng nc nh v sy kh. Nung 600oC n khi than ho hon ton.

    Ho tan cn trong 20 ml dung dch acid nitric 2 M ri lc. Ra cn v phu lc

    bng 15 ml nc. Tp trung dch lc v nc ra, thm nc va 50 ml; thm

    0,5 ml dung dch bc nitrat 0,1 N. Dung dch thu c khng c c hn dung

    dch i chiu c chun b nh sau:

    Ho tan 0,70 g calci carbonat (TT) trong 20 ml dung dch acid nitric 2 M

    (TT) ri lc. Ra cn v phu lc bng 15 ml nc. Tp trung dch lc v nc

    ra; thm 1,2 ml dung dch acid hydrocloric 0,01 N v thm nc va 50 ml.

    Tip tc thm 0,5 ml dung dch bc nitrat 0,1 N.

    Cht kh kali permanganat

    Thm tng git dung dch kali permanganat 0,1 N vo 100 ml nc

    c acid ho bng 1,5 ml dung dch acid sulfuric 10% (TT) ang si n khi mu

    xut hin v bn vng trong 30 giy. Ho tan 1,0 g ch phm trong dung dch

    ang nng trn v chun bng dung dch kali permanganat 0,1 N n khi c

    mu hng bn vng trong 15 giy. Lng dung dch kali permangant 0,1 N tiu

    th khng c qu 0,5 ml.

    Tp cht hu c

    Ho tan 0,50 g ch phm trong 5 ml acid sulfuric m c (TT) v yn

    trong 5 pht. Dung dch thu c khng c c mu thm hn mu ca mu mu

    V5 (Ph lc 5.17, phng php 1).

    Kim loi nng

    Khng c qu 10 phn triu (Ph lc 7.4.7).

  • Ly 12 ml dung dch S v tin hnh th theo phng php 2. Dung dch i

    chiu l dung dch gm 5 ml ethanol 96% (TT) trn u vi 5 ml dung dch ch

    mu 1 phn triu v 2 ml dung dch S.

    Tro sulfat

    Khng c qu 0,1% (Ph lc 7.7, phng php 2).

    Dng 1,0 g ch phm.

    Mt khi lng do lm kh

    Khng c qu 0,5% (Ph lc 5.16).

    (1,000 g; silicagel).

    nh lng

    Ho tan khong 0,200 g ch phm trong 20 ml ethanol 96% (TT) trung

    tnh ho bng dung dch natri hydroxyd 0,1 N vi dung dch phenolphtalein (CT),

    thm 20 ml nc v vi git dung dch phenolphtalein (CT), chun bng dung

    dch natri hydroxyd 0,1 N.

    1 ml dung dch natri hydroxyd 0,1 N tng ng vi 12,21 mg C7H6O2.

    Bo qun

    Ch phm c bo qun trong chai l nt kn.

    Cng dng

    Khng nm, cht bo qun chng vi sinh vt.

    4-ACID CITRIC NGM MT PHN T NC

    Acidum citricum monohydricum

    C6H8O7. H2O P.t.l: 210,1

  • Acid citric ngm mt phn t nc l acid 2 - hydroxypropan - 1,2,3 -

    tricarboxylic, phi cha t 99,5 n 101,0% C6H8O7, tnh theo ch phm khan.

    Tnh cht

    Bt kt tinh trng hoc tinh th hay dng ht khng mu. Ln hoa. Rt d

    tan trong nc, d tan trong ethanol 96%, hi tan trong ether.

    nh tnh

    C th chn mt trong hai nhm nh tnh sau:

    Nhm I: B, E

    Nhm II: A, C, D, E

    A. Ho tan 1 g ch phm trong 10 ml nc, dung dch thu c phi c pH

    nh hn 4 (Ph lc 5.9) B. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph

    hp vi ph hng ngoi ca acid citric monohydrat chun, o sau khi mu th v

    chun c sy 100 n 105oC trong 24 gi.

    C. Thm khong 5 mg ch phm vo hn hp gm 1 ml anhydrid acetic

    (TT) v 3 ml pyridin (TT). Mu xut hin.

    D. Ho tan 0,5 g ch phm trong 5 ml nc, trung ho bng dung dch natri

    hydroxyd 1 M (khong 7 ml), thm 10 ml dung dch calci clorid (TT), un si, kt

    ta trng c to thnh.

    E. Ch phm phi p ng php th nc.

    trong v mu sc ca dung dch

    Ho tan 2,0 g ch phm trong 10 ml nc. Dung dch phi trong (Ph lc

    5.12) v khng c c mu m hn mu mu V7, NV7 hay LV7 (Ph lc 5.17,

    phng php 2).

    Cht d b carbon ho

  • Cho 1,0 g ch phm vo ng nghim, thm 10 ml acid sulfuric (TT), un

    ngay hn hp trong cch thu 900 10C trong 1 gi. Lm ngui tht nhanh,

    dung dch khng c c mu m hn mu ca hn hp gm 1 ml dung dch u

    mu v 9 ml dung dch u mu vng (Ph lc 5.17, phng php 1).

    Acid oxalic

    Trung ho 10 ml dung dch ch phm 10% trong nc bng dung dch

    amoni hydroxyd 6 N (TT), thm 5 git dung dch acid hydrocloric 3 N (TT),

    ngui. Thm 2 ml dung dch calci clorid (TT), dung dch khng c c.

    Sulfat

    Khng c qu 0,015% (Ph lc 7.4.12)

    Ha tan 1,0 g ch phm trong nc c 15 ml v tin hnh th.

    Nhm

    Khng c qu 0,2 phn triu (Ph lc 7.4.8).

    Nu ch phm c dng pha ch dung dch thm phn th phi t php

    th ny.

    Dung dch th: Ho tan 20 g ch phm trong 100 ml nc, thm 10 ml

    dung dch m acetat pH 6,0.

    Dung dch i chiu: Hn hp gm 2 ml dung dch nhm mu 2 phn triu,

    10 ml dung dch m acetat pH 6,0 v 98 ml nc.

    Dung dch mu trng: Hn hp gm 10 ml dung dch m acetat pH 6,0 v

    100 ml nc.

    Kim loi nng

    Khng c qu 10 phn triu (Ph lc 7.4.7).

    Ho tan 5,0 g ch phm lm nhiu ln trong 39 ml dung dch natri

    hydroxyd long (TT), pha long vi nc n 50 ml. Ly 12 ml dung dch ny tin

  • hnh th theo phng php 1. Dng dung dch ch mu 1 phn triu chun b

    mu i chiu.

    Nc

    T 7,5 n 9,0% (Ph lc 6.6).

    Dng 0,500 g ch phm.

    Tro sulfat

    Khng c qu 0,1% (Ph lc 7.7, phng php 2).

    Dng 1,0 g ch phm.

    Ni c t vi khun

    Nu ch phm c dng pha ch cc dng thuc tim phn liu m

    khng c phng php no khc loi ni c t vi khun th ch phm phi

    khng c c vt qu 0,5 n v ni c t cho mi miligam (Ph lc 10.3).

    nh lng

    Ho tan 0,550 g ch phm trong 50 ml nc. Chun bng dung dch

    natri hydroxyd 1 N, dng 0,5 ml dung dch phenolphtalein (CT) lm ch th.

    1 ml dung dch natri hydroxyd 1 N tng ng vi 64,03 mg C6H8O7.

    Bo qun

    Trong l kn.

    5-ACID SALICYLIC

    Acidum salicylicum

    C7H6O3 P.t.l: 138,1

  • Acid salicylic l acid 2 - hydroxybenzencarboxylic, phi cha t 99,0 n

    100,5% C7H6O3, tnh theo ch phm lm kh.

    Tnh cht

    Tinh th hnh kim mu trng hoc khng mu hay bt kt tinh trng. Kh

    tan trong nc, d tan trong ethanol 96% v ether, hi tan trong cloroform. Dung

    dch ch phm c phn ng acid.

    nh tnh

    Chn mt trong hai nhm nh tnh sau:

    Nhm I: A, C

    Nhm II: B, C A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph

    hp vi ph hng ngoi ca acid salicylic chun.

    B. Ho tan 0,01 g ch phm trong 5 ml nc bng cch un nng, ngui.

    Thm 1 git dung dch st (III) clorid 5% (TT) s xut hin mu tm.

    C. im chy: 158 - 161oC (Ph lc 5.19).

    trong v mu sc ca dung dch

    Ho tan 1,0 g ch phm trong 10,0 ml ethanol 96% (TT). Dung dch phi

    trong (Ph lc 5.12) v khng mu (Ph lc 5.17, phng php 2).

    Dung dch S: Ho tan 2,5 g ch phm trong 50 ml nc si, ngui v

    lc.

    Clorid

    Khng c qu 0,010% (Ph lc 7.4.5).

    Ly 10 ml dung dch S pha long thnh 15 ml bng nc v tin hnh th.

    Sulfat

    Khng c qu 0,020% (Ph lc 7.4.12).

  • Ly 15 ml dung dch S v tin hnh th.

    Kim loi nng

    Khng c qu 20 phn triu (Ph lc 7.4.7).

    Ho tan 2,0 g ch phm trong 15 ml ethanol 96% (TT), sau thm 5 ml

    nc. Ly 12 ml dung dch ny th theo phng php 2. Dng dung dch ch mu

    100 phn triu pha long bng hn hp dung mi ethanol 96% - nc (3: 1)

    c dung dch ch mu 2 phn triu dng chun b mu i chiu.

    Mt khi lng do lm kh

    Khng c qu 0,5% (Ph lc 5.16).

    (1,000 g; p sut gim; silicagel).

    Tro sulfat

    Khng c qu 0,1% (Ph lc 7.7, phng php 2).

    Dng 2,0 g ch phm.

    nh lng

    Ho tan khong 0,250 g ch phm trong 25 ml ethanol 96% (TT) c

    trung tnh ho bng dung dch natri hydroxyd 0,1 N vi dung dch phenolphtalein

    (CT), thm 20 ml nc v vi git dung dch phenolphtalein (CT). Chun bng

    dung dch natri hydroxyd 0,1 N.

    1 ml dung dch natri hydroxyd 0,1 N tng ng vi 13,81 mg C7H6O3.

    Bo qun

    Ch phm c bo qun trong chai l nt kn, trnh nh sng.

    6-AMINOPHYLIN

    Aminophyllinum

    Theophylin v ethylendiamin

  • (C7H8 N4O2)2. C2H8 N2

    P.t.l: 420,4 (Aminophylin khan)

    (C7H8 N4O2)2. C2H8 N2. 2H2O P.t.l: 456,6 (Aminophylin

    dihydrat)

    Aminophylin l hn hp n nh ca theophylin v ethylendiamin. Ch

    phm c th khan hoc ngm khng nhiu hn hai phn t nc, phi cha t 84,0

    n 87,4% C7H8 N4O2 v t 13,5 n 15,0% C2H8 N2, tnh theo ch phm khan.

    Tnh cht

    Bt trng hay hi vng, hoc ht nh, thong mi amoniac, v ng. Di

    tc dng ca khng kh m, nh sng, nhit cao, aminophylin b bin mu.

    ngoi khng kh aminophylin t t b mt ethylendiamin, ng thi hp thu carbon

    dioxyd, gii phng theophylin t do. ni thiu nh sng, n b phn hu t t khi

    tip xc vi khng kh m. S phn hu xy ra nhanh hn nhit cao.

    D tan trong nc (dung dch c th tr nn c khi hp thu carbon

    dioxyd), thc t khng tan trong ethanol v ether.

    nh tnh

    C th chn mt trong hai nhm nh tnh sau:

    Nhm I: B, C, E.

    Nhm II: A, C, D, E, F.

  • Ho tan 1,0 g ch phm trong 10 ml nc , thm tng git 2 ml dung dch

    acid hydrocloric long (TT) v lc, lc. Ta dng lm nh tnh A, B, D v F.

    Dch lc dng lm nh tnh C.

    A. Ta c ra bng nc v sy kh 100 n 105oC, c im chy t

    270 n 274oC (Ph lc 5.19).

    B. Ph hng ngoi (Ph lc 3.2) ca ta c ra bng nc v sy kh

    100 n 105oC phi ph hp vi ph hng ngoi i chiu ca theophylin hoc

    ph hng ngoi ca theophylin chun.

    C. Thm 0,2 ml benzoyl clorid (TT) vo dch lc. Kim ho bng dung dch

    natri hydroxyd long (TT) v lc k. Lc ly ta, ra bng 10 ml nc , ha tan

    trong 5 ml ethanol 96% (TT) nng ri thm 5 ml nc. Ta to thnh, sau khi

    c ra v sy kh 100 n 105oC, c im chy t 248 n 252oC (Ph lc

    5.19).

    D. Ho tan khong 10 mg ta trong 10 ml nc, thm 0,5 ml dung dch

    thu ngn (II) acetat 5% v yn, s xut hin ta tinh th trng.

    E. Phi p ng php th nc (xem php th nc).

    F. Ta cho phn ng ca nhm xanthin (Ph lc 7.1).

    trong v mu sc ca dung dch

    Ho tan 0,5 g ch phm trong 10 ml nc khng c carbon dioxyd (TT)

    bng cch un nng. Dung dch khng c c hn c mu S2 (Ph lc

    5.12) v khng c m mu hn mu mu LV6 (Ph lc 5.17, phng php 2).

    Kim loi nng

    Khng c qu 20 phn triu (Ph lc 7.4.7).

    Ly 1,0 g ch phm th theo phng php 3. Dng 2 ml dung dch ch mu

    10 phn triu chun b mu i chiu.

  • Tp cht lin quan

    Khng c qu 0,5%.

    Tin hnh theo phng php sc k lp mng (Ph lc 4.4).

    Bn mng: Silicagel GF254

    Dung mi khai trin: Amoniac m c - aceton - cloroform - butanol (10:

    30: 30: 40). Dung dch th: Ho tan 0,2 g ch phm trong 2 ml nc bng cch

    un nng v pha long ti 10 ml bng methanol (TT).

    Dung dch i chiu: Pha long 0,5 ml dung dch th ti 100 ml bng

    methanol (TT).

    Cch tin hnh: Chm ring bit ln bn mng 10 l mi dung dch trn.

    Trin khai bn mng ti khi dung mi i c khong 15 cm. kh bn mng

    ngoi khng kh, v quan st di nh sng t ngoi bc sng 254 nm. Trn

    sc k ca dung dch th ngoi vt chnh bt k vt ph no xut hin u

    khng c m mu hn vt ca dung dch i chiu.

    Nc

    Khng c qu 1,5% (i vi dng khan) (Ph lc 6.6). Xc nh trn

    2,000 g ch phm ho tan trong 20 ml pyridin khan (TT). T 3,0 n 8,0% (i

    vi dng ngm nc) (Ph lc 6.6). Xc nh trn 0,500 g ch phm ho tan trong

    20 ml pyridin khan (TT).

    Tro sulfat

    Khng c qu 0,1% (Ph lc 7.7, phng php 2).

    Dng 1,0 g ch phm.

    nh lng

  • Ethylendiamin: Ho tan 0,250 g ch phm trong 30 ml nc, thm 0,1 ml

    dung dch lc bromocresol (CT1). Chun bng dung dch acid hydrocloric 0,1

    M cho ti khi xut hin mu xanh lc.

    1 ml dung dch acid hydrocloric 0,1 M tng ng vi 3,005 mg C2H8

    N2.

    Theophylin: Sy khong 0,200 g ch phm 135oC n khi lng khng

    i. Ho tan cn trong 100 ml nc bng cch un nng, ngui, thm 20 ml

    dung dch bc nitrat 0,1 N v lc. Thm 1 ml dung dch xanh bromothymol (CT)

    v chun bng dung dch natri hydroxyd 0,1 M cho ti khi c mu xanh l.

    1 ml dung dch natri hydroxyd 0,1 M tng ng vi 18,02 mg C7H8

    N4O2.

    Bo qun

    Trong chai l nt kn, trnh nh sng.

    Ch phm

    Thuc tim aminophylin. Vin nn aminophylin

    Tc dng v cng dng

    Gin kh - ph qun, gin c trn mch mu, li tiu. Tr hen suyn.

    7-AMPICILIN

    Ampicillinum

    C16H19 N3O4S P.t.l: 349,40

    Ampicilin l acid (6R) -6 -( - D - phenylglycylamino) penicilanic, phi

    cha t 96,0 n 100,5% C16H19 N3O4S, tnh theo ch phm khan.

  • Tnh cht

    Bt kt tinh trng, khng mi hoc hu nh khng mi.

    Hi tan trong nc, thc t khng tan trong ethanol, cloroform, ether, du

    bo. Tan trong dung dch acid long v dung dch hydroxyd kim.

    nh tnh

    C th chn mt trong hai nhm nh tnh sau:

    Nhm I: A, D

    Nhm II: B, C, D

    A. Ph hng ngoi (Ph lc 3.2) ca ch phm phi ph hp vi ph hng

    ngoi ca ampicilin chun.

    B. Tin hnh phng php sc k lp mng theo nh tnh cc penicilin

    (Ph lc 7. 2).

    Dng pha ng B.

    C. Phn ng B trong php th phn ng mu ca cc penicilin v

    cephalosporin (Ph lc 7. 3).

    D. Phi p ng php th nc (xem php th nc).

    pH

    T 3,5 n 5,5 (Ph lc 5.9).

    Xc nh trn dung dch ch phm 0,25% trong nc khng c carbon

    dioxyd (TT).

    trong ca dung dch

    Ho tan 1,0 g ch phm trong 10 ml dung dch acid hydrocloric 1 M, ng

    thi ho tan 1,0 g ch phm trong 10 ml dung dch amoniac 2 M. Quan st ngay