CAMPHOR

Camphora

Long nao

 

 

 

va chat ong phan oi anh

 

 

C10H16O P.t.l: 152,2

Camphor la (1RS,4SR)-1,7,7-trimethylbicyclo-[2.2.1] heptan-2-on, ược chiet t tinh dau cua cay Long nao Cinnamomum camphora (Linn.) Nees et Eberm, ho Lauraceae (camphor thien nhien, hu tuyen) hoac c ieu che bang tong hp hoa hoc (camphor tong hp, racemic hoac ta tuyen).

Tnh chat

Bot ket tinh trang hoac phien, khoi ket tinh khong mau. De nghien mn vi mot t ethanol, cloroform hay ether. Mui thm manh, ac trng; v luc au nong sau mat lanh va de chu; de thang hoa ngay nhiet o thng. un nong can than, che pham thang hoa hoan toan va khong b carbon hoa; chay cho khoi en va ngon la sang.

Kho tan trong nc, rat tan trong cloroform, ethanol 96%, ether, ether dau hoa, de tan trong dau beo va tinh dau, rat t tan trong glycerin.

nh tnh

Co the chon mot trong hai nhom nh tnh sau:

Nhom I: A, C.

Nhom II: A, B, D.

Dung dch S: Hoa tan 2,50 g che pham trong 10 ml ethanol 96% (TT) va pha long thanh 25,0 ml vi cung dung moi.

A. Goc quay cc rieng. Xac nh tren dung dch S (Phu luc 6.4).

Camphor thien nhien (loai hu tuyen): T +39 en +44o.

Camphor tong hp (loai racemic): T -1,5 en +1,5o; (loai ta tuyen): T -39 en -44o.

B. iem chay: Camphor thien nhien chay 174 en 181 oC; Camphor tong hp chay 172 en 180 oC (Phu luc 6.7).

C. Pho hong ngoai cua che pham (Phu luc 4.2) phu hp vi pho hong ngoai oi chieu cua camphor hoac pho hong ngoai cua camphor chuan (ĐC). Tien hanh th che pham di dang bot nhao vi parafin long (TT).

D. Pha loang 0,5 ml dung dch S vi ethanol 96% (TT) thanh 20 ml. o pho hap thu t ngoai (Phu luc 4.1) trong khoang bc song từ 230 đến 350 nm. Dung dch co mot cc ai hap thu 289 nm va o hap thu 289 nm khoang 0,53.

Khi tien hanh cac phep th can can che pham can than va hoa tan nhanh.

o trong va mau sac cua dung dch

Dung dch S phai trong (Phu luc 9.2) va khong mau (Phu luc 9.3 phng phap 2).

Gii han acid - kiem

Them 0,1 ml dung dch phenolphtalein (TT) vao 10 ml dung dch S, dung dch phai khong mau. Mau phai chuyen sang hong, khi them khong qua 0,2 ml dung dch natri hydroxyd 0,1 N (C).

Tap chat lien quan

Tien hanh bang phng phap sac ky kh ( phu luc 5.2)

Dung dch th: Hoa tan 2,50 g che pham trong heptan (TT) va pha loang thanh 25 ml vi cung dung moi

Dung dch oi chieu (1): Pha loang 1,0 ml dung dch th thanh 100,0 ml vi heptan (TT).

Dung dch oi chieu (2): Pha loang 10,0 ml dung dch oi chieu (1) thanh 20,0 ml vi heptan (TT).

Dung dch oi chieu (3): Hoa tan 0,50 g borneol (TT) trong heptan (TT) va pha loang thanh 25 ml vi cung dung moi. Pha loang 5,0 ml dung dch tren thanh 50,0 ml vi heptan (TT).

Dung dch phan giai: Hoa tan 50 mg linalol (TT) va 50 mg bornyl acetat (TT) trong heptan (TT) va pha loang ti 100 ml vi cung dung moi.

ieu kien sac ky:

Cot: (30 m x 0,25 mm) c nhoi macrogol 20 000 ( 0,25 m) (TT).

Kh mang: Heli dung cho sac ky.

Ty le chia dong: 1 : 70

Toc o dong: 45 cm/s.

Nhiet o:

 

 

Thi gian

(phut)

Nhiet o

(oC)

Cot

0 - 10

50

 

10 - 35

50 100

 

35 - 45

100 200

 

45 - 55

200

Buong tiem

 

220

Detector

 

250

Detector: Ion hoa ngon la

The tch tiem : 1 l

Cach tien hanh:

Tiem dung dch phan giai: phep th ch co gia tr khi o phan giai gia 2 pic bornyl acetat va linalol t nhat la 3,0.

Tiem cac dung dch oi chieu va dung dch th. Tren sac ky o cua dung dch th:

Dien tch pic tng ng borneol khong c ln hn dien tch pic chnh tren sac ky o cua dung dch oi chieu 3 (2,0%). Dien tch cua bat ky pic phu nao khac ngoai pic tng ng borneol va pic chnh, khong c ln hn 0,5 lan dien tch pic chnh tren sac ky o cua dung dch oi chieu (1) (0,5%).

Tong dien tch pic cua cac pic phu khac khong c ln hn 4 lan dien tch pic chnh tren sac ky o cua dung dch oi chieu 1 (4,0%)

Bo qua cac pic co dien tch nho hn: 0,1 lan dien tch pic chnh tren sac ky o cua dung dch oi chieu 2 ( 0,05%)

Halogen

Khong c qua 0,01% (Phu luc 9.4.5).

Hoa tan 1,0 g che pham trong 10 ml 2-propanol (TT) trong bnh chng cat. Them 1,5 ml dung dch natri hydroxyd 2 M (TT), 50 mg hp kim nhom - nickel (TT). un cach thuy en khi 2-propanol bay hi hoan toan. e nguoi va them 5 ml nc. Khuay eu va loc qua giay loc t a c ra bang nc en khi het clorid. Pha loang dch loc thanh 10,0 ml vi nc. Them vao 5,0 ml dung dch tren tng giot acid niric (TT) en khi tua tao thanh tan tr lai va pha loang thanh 15 ml vi nc. Dung dch thu c ap ng phep th gii han clorid.

Nc

Hoa tan 1 g che pham trong 10 ml ether dau hoa (TT). Dung dch phai trong (Phu luc 9.2).

Can sau khi boc hi

Khong c qua 0,05%.

Boc hi 2,0 g che pham tren cach thuy va say kho 100 en 105 oC trong 1 gi. Can con lai khong c qua 1 mg.

Bao quan

Trong chai lo nut kn, e ni kho mat.

Ghi chu

Tng k: Tao hon hp chay long (hon hp long, ac set, trong suot) vi phenol, menthol, thymol, salol, naphthol, resorcin, pyrocatechol, pyrogalol, acid salicylic, phenylsalicylat, cloral hydrat, antipirin ...

Loai thuoc

Thuoc kch thch da, giam au, chong nga.

Che pham

Con long nao, con long nao - opi, nc long nao am ac, dau xoa long nao.