BARBITURAT

Mikhania C.E., M.Si, Apt

 PENDAHULUAN
• Senyawa barbiturat adalah senyawa turunan
asam barbiturat
• Digunakan sebagai depresan saraf pusat 
anastesi dan sedasi
• Struktur dasar : asam barbiturat
 SIFAT-SIFAT
1. Umumnya berupa zat padat, kristal putih/tidak
berwarna dan rasanya sedikit pahit
2. Tidak larut dalam air (bentuk keto) tapi mudah larut
dalam CHCl3, eter dan lain-lain
3. Bereaksi asam lemah dan dapat membentuk garam
yang larut dalam air, misalnya dengan NaOH dan KOH
4. Larutan garam Na/K dalam air tidak stabil dalam
pemanasan
 PEMBAGIAN

KLASIFIKASI LAMA KERJA (Jam) CONTOH

Ultra short acting 3–4 Tiopental

Short acting 4 - 10 Pentobarbital

Long acting 8 - 24 Fenobarbital, barbital

 Identifikasi
• Jarak lebur
• KLT
• Spektrofotometri IR
• Reaksi warna
• Bentuk kristal
 1. FENOBARBITAL

• Pemerian : A white or almost white, crystalline powder or

colourless crystals

• Kelarutan : very slightly soluble in water, freely soluble in

alcohol. It forms water-soluble compounds with alkali hydroxides
and carbonates and with ammonia.
 Identifikasi
Reaksi Pendahuluan

Reaksi Parri : zat dalam larutan methanol +

pereaksi parri + NH4OH akan terjadi perubahan
warna.
 Identifikasi (cont.)
Reaksi Penegasan
• Reaksi zwikker (zat dalam larutan methanol/etanol +
pereaksi zwikker akan terbentuk warna violet
• Zat + air + larutan AgNO3 terbentuk warna putih
• Zat + Merkurium Nitrat terbentuk warna hitam
• Zat + H2SO4 pekat + α naftol terbentuk warna ungu
• Zat + Formalin + H2SO4 pekat terbentuk warna merah

Reaksi Kristal
• Sampel + aseton + air
• Sampel + Fe Complex
• Sampel + Cu Complex
 Identifikasi (cont.)
A. Determine the melting point of the substance to be examined. Mix
equal parts of the substance to be examined and phenobarbital CRS
and determine the melting point of the mixture. The difference
between the melting points (which are about 176 °C) is notgreater
than 2 °C.
B. Examine by infrared absorption spectrophotometry comparing with
the spectrum obtained with phenobarbital CRS.
C. Examine by thin-layer chromatography, using silica gel GF254 R as the
coating substance.
• Test solution : Dissolve 0.1 g of the substance to be examined in alcohol
R and dilute to 100 ml with the same solvent.
• Reference solution : Dissolve 0.1 g of phenobarbital CRS in alcohol R and
dilute to 100 ml with the same solvent.
• Apply separately to the plate 10 μl of each solution. Develop over a path
of 18 cm using the lower layer of a mixture of 5 volumes of
concentrated ammonia R, 15 volumes of alcohol R and 80 volumes of
chloroform R. Examine immediately in ultraviolet light at 254 nm. The
principal spot in the chromatogram obtained with the test solution is
similar in position and size to the principal spot in the chromatogram
obtained with the reference solution.
 2. PENTOBARBITAL

• Pemerian : A white or almost white, crystalline

powder or colourless crystals
• Kelarutan : very slightly soluble in water, freely
soluble in ethanol. It forms water-soluble
compounds with alkali hydroxides and
carbonates and with ammonia.
 Identifikasi
A. Determine the melting point of the substance to be examined. Mix equal parts
of the substance to be examined and pentobarbital CRS and determine the
melting point of the mixture. The difference between the melting points
(which are about 133 °C) is not greater than 2 °C.
B. Examine by thin-layer chromatography (2.2.27), using silica gel GF254 R as the
coating substance.
• Test solution : Dissolve 0.1 g of the substance to be examined in alcohol R and
dilute to 100 ml with the same solvent.
• Reference solution : Dissolve 0.1 g of pentobarbital CRS in alcohol R and dilute to
100 ml with the same solvent. Apply to the plate 10 μl of each solution. Develop
over a path of 18 cm using the lower layer of a mixture of 5 volumes of
concentrated ammonia R, 15 volumes of alcohol R and 80 volumes of chloroform
R.
• Examine immediately in ultraviolet light at 254 nm. The principal spot in the
chromatogram obtained with the test solution is similar in position and size to
the principal spot in the chromatogram obtained with the reference solution.
C. To about 10 mg add about 10 mg of vanillin R and 2 ml of sulphuric acid R. Mix
and heat on a water-bath for 2 min. A reddish-brown colour develops. Cool and
add cautiously 5 ml of ethanol R. The colour becomes violet and then blue.
 3. AMOBARBITAL

• Pemerian : A white or almost white, crystalline

powder
• Kelarutan : very slightly soluble in water, freely
soluble in alcohol, soluble in methylene chloride.
It forms water-soluble compounds with alkali
hydroxides and carbonates and with ammonia.
 Identifikasi
A. Determine the melting point of the substance
to be examined. Mix equal parts of the
substance to be examined and amobarbital CRS
and determine the melting point of the mixture.
The difference between the melting points
(which are about 157 °C) is not greater than 2
°C.
B. Examine by infrared absorption
spectrophotometry comparing with the
spectrum obtained with amobarbital CRS .
 Identifikasi (Cont.)
C. Examine by thin-layer chromatography, using silica gel GF254 R as
the coating substance.
• Test solution : Dissolve 0.1 g of the substance to be examined in
alcohol R and dilute to 100 ml with the same solvent.
• Reference solution : Dissolve 0.1 g of amobarbital CRS in alcohol R
and dilute to 100 ml with the same solvent.
• Apply separately to the plate 10 μl of each solution. Develop over a
path of 18 cm using the lower layer from a mixture of 5 volumes of
concentrated ammonia R, 15 volumes of alcohol R and 80 volumes
of chloroform R. Examine immediately in ultraviolet light at 254 nm.
The principal spot in the chromatogram obtained with the test
solution is similar in position and size to the principal spot in the
chromatogram obtained with the reference solution.

D. It gives the reaction of non-nitrogen substituted barbiturates

 SPEKTRUM IR
• Fenobarbital
 Spektrum IR
• Pentobarbital