PHYTOMENADION

Phytomenadionum

Vitamin K1

 

 

 

 

 

 

 

 

 

 

C31H46O2 P.t.l: 450,71

Phytomenadion la hon hp cua 2-methyl-3-[(2E)-(7R,11R)-3,7,11,15-tetramethylhexadec-2-enyl]naphthalen-1,4-dion (trans-phytomenadion), 2-methyl-3-[(2Z)-(7R,11R)-3,7,11,15-tetramethylhexadec-2-enyl]naphthalen-1,4-dion (cis-phyto menadion) va 2,3-epoxy-2-methyl-3-[(2E)-(7R,11R)-3,7,11,15-tetramethyl hexadec-2-enyl]-2,3-dihydronaphthalen-1,4-dion (trans-epoxyphytomenadion). Cha khong qua 4,0% trans-epoxyphytomenadion va khong t hn 75,0% trans-phytomenadion. Tong cua 3 thanh phan khong c t hn 97,0% va khong c nhieu hn 103,0%

Tnh chat

Chat long dang dau nht, trong va mau vang hoac vang cam, khong mui.

De tan trong ether, iso octan, cloroform va dau beo.

Hi tan trong ethanol va methanol, thc te khong tan trong nc. No b phan huy dan dan va b sam mau do anh sang.

Ch so khuc xa khoang 1,526.

nh tnh

Tien hanh nhanh chong va tranh tac ong cua anh sang

A. Hoa tan 10,0 mg che pham trong trimethylpentan (TT) va pha loang thanh 100,0 ml vi cung dung moi. Pho t ngoai ( phu luc 4.1) cua dung dch thu c trong vung t 275 nm en 340 nm cho hap thu cc ai 327 nm va cc tieu 285 nm. A (1%; 1 cm) bc song cc ai phai t 67 en 73.

Pha loang tiep 10,0 ml dung dch tren thanh 50,0 ml vi trimethylpentan. Pho t ngoai (Phu luc 4.1) cua dung dch nay trong vung t 230 nm en 280 nm, cho 4 hap thu cc ai 243 nm, 249 nm, 261 nm va 270 nm

B. Trong sac ky o th Menadion va tap chat lien quan khac: Vet chnh cua dung dch th (2) phai tng t ve v tr, mau sac va kch thc vi vet chnh cua dung dch oi chieu (1)

C. Hoa tan 50 mg che pham trong 10 ml methanol (TT) va them 1 ml dung dch kali hydroxyd 20% trong methanol (TT) mau xanh luc xuat hien va tr nen tm o khi un nong trong cach thuy 40 oC va sau o chuyen sang mau nau o.

o trong cua dung dch

Hoa tan 2,5 g che pham trong trimethylpentan va pha loang thanh 25 ml vi cung dung moi. Dung dch phai trong (Phu luc 9.2).

Ch so acid

Khong qua 2,0 (phu luc 7.2) ( dung 2,00 g che pham.)

Menadion va cac tap chat lien quan khac

Xac nh bang phng phap sac ky lp mong (phu luc 5.4)

Ban mong: Silica gel GF254 (TT)

Dung moi khai trien: Cyclohexan - toluen (20 : 80)

Dung dch th (1)

Hoa tan 0,40 g che pham trong cyclohexan (TT) va pha loang thanh 10 ml vi cung dung moi

Dung dch th (2)

Pha loang 1 ml dung dch th (1) thanh 10 ml vi cyclohexan (TT) .

Dung dch oi chieu (1)

Hoa tan 40 mg phytomenadion chuan (C) trong cyclohexan (TT) va pha loang thanh 10 ml vi cung dung moi

Dung dch oi chieu (2)

Pha loang 1 ml dung dch th (2) thanh 20 ml bang cyclohexan (TT)

Dung dch oi chieu (3)

Hoa tan 4,0 mg menadion (TT) trong cyclohexan (TT) va pha loang thanh 50 ml vi cung dung moi

Cach tien hanh: Cham rieng biet len ban mong 10 ml moi dung dch tren. Trien khai sac ky en khi dung moi i c khoang 15 cm, lay ban mong ra, e kho ngoai khong kh trong 5 phut. Quan sat di anh sang t ngoai bc song 254 nm va phun dung dch acid phosphomolybdic 10% trong ethanol (TT). Say ban mong 120 oC trong 5 phut.

Quan sat di anh sang thng. Tren sac ky o cua dung dch th (1):

Bat c vet nao tng ng menadion khong c am mau hn vet tren sac ky o cua dung dch oi chieu (3) (0,2%); Bat c vet nao, khac vet chnh va vet tng ng mennadion, khong c am mau hn vet cua dung dch oi chieu (2) (0,5%). Khong Bo qua bat c vet nao nam di vet chnh va khong tach hoan toan khoi vet chnh.

Tro sulfat

Khong c qua 0,1 % ( Phu luc 9.9, phng phap 2).

Dung 1,0 g che pham

nh lng

Phng phap sac ky long (Phu luc 5.3).

Pha ong : Octanol - di-isopropyl ether - heptan (0,67 : 3,3 : 1000)

Dung dch th

Hoa tan 15,0 mg che pham trong pha ong va pha loang thanh 10,0 ml vi pha ong.

Dung dch oi chieu (1)

Hoa tan 15,0 mg phytomenadion chuan (C) trong pha ong va pha loang thanh 10,0 ml vi pha ong.

Dung dch oi chieu (2)

Hoa tan 15,0 mg phytomenadion chuan (C) va 4,0 mg trans-epoxyphytomenadion chuan (C) trong pha ong va pha loang thanh 10,0 ml vi pha ong.

ieu kien sac ky:

Cot thep khong r 0,25 m x 4,6 mm c nhoi spherical silica gel dung cho sac ky (5 mm) vi lo xop 8 nm.

Toc o dong: 0,4 ml/phut

Detector quang pho t ngoai at tai bc song 254 nm.

The tch tiem: 20 ml.

Tiem dung dch oi chieu (2). ieu chnh o nhay cua he thong sao cho chieu cao cua pic chnh t nhat bang 50% cua thang o.

Phep th ch co gia tr khi th t ra giai cua cac pic la trans-epoxyphytomenadion, cis-phytomenadion va trans-phytomenadion. Tien hanh tiem dung dch oi chieu (1) 6 lan. Phep nh lng ch co gia tr khi o lech chuan tng oi dien tch pic ong phan trans nho hn 1,0% va o phan giai gia pic tng ng trans-phytomenadion va cis-phytomenadion t nhat la 2,5. Tiem dung dch th va dung dch oi chieu, tnh toan nong o phan tram cua trans-phytomenadion, cis-phytomenadion va trans-epoxyphytomenadion theo cac cong thc sau:

 

m' x A'trans x Strans

Trans-phytomenadion =

m x S'trans

m' x A'cis x Scis

Cis-phytomenadion =

m x S'cis

m' x A'epoxy x Sepoxy

trans epoxyphytomenadion

m x S'epoxy

m' = Khoi lng (mg) chat chuan trong dung dch oi chieu (1)

m = Khoi lng (mg) che pham trong dung dch th

Atrans = Ham lng (%) trans-phytomenadion trong phytomenadion chuan

Acis = Ham lng (%) cis-phytomenadion trong phytomenadion chuan

Aepoxy = Ham lng (%) trans - epoxyphytomenadion trong phytomenadion chuan

Strans = Dien tch pic tng ng vi ong phan trans trong sac ky o cua dung

dch th

Scis = Dien tch pic tng ng vi ong phan cis trong sac ky o cua dung dch

th

Sepoxy = Dien tch pic tng ng vi ong phan trans epoxyphytomenadion -

trong sac ky o cua dung dch th

Strans = Dien tch pic tng ng vi ong phan tran trong sac ky o cua dung dch oi chieu (1)

Scis = Dien tch pic tng ng vi ong phan cis trong sac ky o cua dung

dch oi chieu (1)

Sepoxy = Dien tch pic tng ng vi ong phan trans-epoxyphytomenadion

trong sac ky o cua dung dch oi chieu (1)

Bao quan

Trong bao b kn, tranh anh sang.

Loai thuoc

Tng t vitamin K.

Che pham

Thuoc tiem, vien nen.