Karakterisasi Simplisia Dan Isolasi Minyak Atsiri Dari Kulit Buah Jeruk Jingga (Citrus x Jambhiri Lush) Segar Dan Kering Serta Analisis Komponennya Secara GC-MS

Lampiran 1. Hasil identifikasi tumbuhan jeruk jingga (Citrus x jambhiri Lush)

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Lampiran 2. Gambar tumbuhan jeruk jingga dan buah jeruk jingga

A

a

b

Keterangan:
a. Tumbuhan jeruk jingga
b. Buah jeruk jingga

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Lampiran 3. Kulit buah jeruk jingga segar dan kering dan serbuk simplisia jeruk
jingga

a
a

b

c

Keterangan:
a. Kulit jeruk jingga segar
b. Simplisia kulit jeruk jingga (Citri jambhirii pericarpium)
c. Serbuk kulit jeruk jingga

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Lampiran 4. Alat–alat yang digunakan

Gambar alat penetapan kadar air

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Gambar alat penetapan kadar minyak atsiri
Lampiran 4. (Lanjutan)

Gambar alat destilasi air

Gambar Refraktometer Abbe

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Lampiran 4. (Lanjutan)

Gambar piknometer

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Gambar Gas Chromatograph– Mass Spectrometer
Lampiran 5. Hasil pemeriksaan mikroskopik serbuk simplisia kulit buah jeruk
jingga (perbesaran 10x40)

1

2

3
4

Keterangan :
1.
rongga minyak skizolisigen
2.
dengan kristal kalsium oksalat bentuk prisma
3.
pembuluh
4. Parenkim

Fragmen
Parenkim
Berkas

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Lampiran 6. Penetapan kadar air

=

Kadar air
a.

Berat sampel = 5,0090 g
Volume I

= 0,1 ml

Volume II

= 0,5 ml

Kadar air

=

b. Berat sampel

= 5,0080 g

Volume I

= 0,5 ml

Volume II

= 0,9 ml

Kadar air

=

c.

= 7,98%

x 100% = 7,98%

Berat sampel = 5,0020 g
Volume I

= 0,9 ml

Volume II

= 1,3 ml

Kadar air

=

Kadar air rata-rata

=

x 100% = 7,99%

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Lampiran 7. Penetapan kadar sari yang larut dalam air

a.

b.

c.

Berat sampel = 5,0020 g
Berat sari

= 0,2017 g

Kadar sari

=

100% = 20,16%

Berat sampel = 5,0020 g
Berat sari

= 0,2028 g

Kadar sari

=

100% = 20,27%

Berat sampel = 5,0020 g
Berat sari

= 0,2004

Kadar sari

=

Kadar sari rata-rata

=

100% = 20,03%
= 20,15%

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Lampiran 8. Penetapan kadar sari yang larut dalam etanol

a.

b.

c.

Berat sampel = 5,0080 g

Berat sari

= 0,1116 g

Kadar sari

=

100% =10,04%

Berat sampel = 5,0010g
Berat sari

= 0,1079 g

Kadar sari

=

100% = 10,79%

Berat sampel = 5,0010 g
Berat sari

= 0, 1081 g

Kadar sari

=

100% = 10,81%

=

= 10,91%

Kadar sari rata-rata

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Lampiran 9. Penetapan kadar abu total

a.

b.

c.

Berat sampel = 2,0090 g
Berat abu

= 0,075 g

Kadar abu

=

100 % = 3,73 %

Berat sampel = 2,0000 g
Berat abu

= 0,0728 g

Kadar abu

=

100% = 3,64%

Berat sampel = 2,0002 g
Berat abu

= 0,0725 g

Kadar abu

=

Kadar abu total rata-rata =

100% = 3,62%

= 3,66%

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Lampiran 10. Penetapan kadar abu yang tidak larut dalam asam
Kadar abu yang tidak larut dalam asam
Sampel I

x 100%

=

Berat sampel = 2,009 g
Berat abu

= 0,017g

Kadar abu

=

x 100%

= 0,85 %
Sampel II

Berat sampel = 2,000 g
Berat abu

= 0,017 g

Kadar abu

=

x 100%

= 0,85 %
Sampel III

Berat sampel = 2,001 g
Beratabu

= 0,017 g

Kadar abu

=
= 0,85 %

Kadar abu yang tidak larut dalam asam rata-rata =
= 0,85%

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Lampiran 11. Penetapan kadar minyak atsiri kulit buah jeruk jingga
a. Kadar minyak atsiri kulit jeruk jingga segar
Kadar minyak atsiri

=

Sampel I
Volume minyak atsiri = 0,42 ml
Berat sampel

= 10,0850 g

Kadar minyak atsiri

=

= 4,16 %

Sampel II
Volume minyak atsiri = 0,42 ml
Berat sampel

= 10,0660 g

Kadar minyak atsiri

=
= 4,17%

Sampel III
Volume minyak atsiri = 0,42 ml
Berat sampel

= 10,0320 g

Kadar minyak atsiri =
= 4,18%

Kadar minyak atsiri rata-rata

=

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= 4,17%
b. Kadar minyak atsiri kulit buah jeruk jingga kering
Kadar minyak atsiri

=

Sampel I
Volume minyak atsiri = 0,8 ml
Berat sampel

= 10,0140 g

Kadar minyak atsiri

=
= 7,98 %

Sampel II
Volume minyak atsiri = 0,8 ml
Berat sampel

= 10,0250 g

Kadar minyak atsiri

=
= 7,98 %

Sampel III
Volume minyak atsiri = 0,8 ml
Berat sampel

= 10,0510 g

Kadar minyak atsiri =
= 7,96 %

Kadar minyak atsiri rata-rata

=

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= 7,97 %
Lampiran 12. Penetapan indeks bias minyak atsiri simplisia kulit jeruk jingga
segar
a. Indeks bias minyak atsiri simplisia kulit jeruk jingga segar
Sampel I

= 1,4245

Sampel II

= 1,4245

Sampel III

= 1,4245

Indeks bias rata-rata =
= 1,4245

b. Indeks bias minyak atsiri simplisia kulit jeruk jingga kering
Sampel I

= 1,4240

Sampel II

= 1,4240

Sampel III

= 1,4240

Indeks bias rata-rata =
= 1,4240

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Lampiran 13. Penetapan bobot jenis minyak atsiri simplisia kulit jeruk jingga
a. Bobot jenis minyak atsiri simplisia kulit jeruk jingga segar
Sampel I
Bobot piknometer kosong

= 8,5415

Bobot piknometer + air suling

= 10,5418

Bobot piknometer + minyak atsiri

= 10,2471

Bobot jenis minyak atsiri

=

= 0,8526

Sampel II
Bobot piknometer kosong

= 8,5415

Bobot piknometer + air suling

= 10,5418

Bobot piknometer + minyakatsiri

= 10,2470

Bobot jenis minyak atsiri

=

= 0,8526

Sampel III
Bobot piknometer kosong

= 8,5415

Bobot piknometer + air suling

= 10,5418

Bobot piknometer + minyak atsiri

= 10,2478

Bobot jenis minyak atsiri

=

Bobot jenis rata-rata

=

= 0,8530

= 0,8527

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b. Bobot jenis minyak atsiri simplisia kulit jeruk jingga segar
Sampel I
Bobot piknometer kosong

= 8,5415

Bobot piknometer + air suling

= 10,5418

Bobot piknometer + minyak atsiri

= 10,2477

Bobot jenis minyak atsiri

=
= 0,8529

Sampel II
Bobot piknometer kosong

= 8,5415

Bobotpiknometer + air suling

= 10,5418

Bobot piknometer + minyak atsiri

= 10,2470

Bobot jenis minyak atsiri

=
= 0,8526

Sampel III
Bobot piknometer kosong

= 8,5415

Bobot piknometer + air suling

= 10,5418

Bobot piknometer + minyak atsiri

= 10,2470

Bobot jenis minyak atsiri

=
= 0,8526

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Bobot jenis rata-rata

=

= 0,8527

Lampiran 14. Flowsheet isolasi minyak atsiri kulit buah jeruk jingga (Citrus x
jambhiri Lush)
Kulit buah jeruk jingga
dibersihkan
dikeringkan
Simplisia
dihaluskan
di destilasi air*
Serbuk Simplisia

Minyak Atsiri dan Air

di karakterisasi
1. Mikroskopis
2. PK Air
3. PK Abu
• Total
• Tidak Larut Asam
4. PK Sari
• Larut air
• Larut etanol
5. PK Minyak Atsiri

dipisahkan
Minyak atsiri dengan
kemungkinan adanya air

Air

di tambah Na2SO4 anhidrat
Minyak atsiri

Na2SO4 x H2O

di identifikasi

Secara Fisika

Secara Fisikokimia
dengan GC-MS

Indeks Bias

Bobot Jenis

Kromatogram
GC

Spektrum
MS

Keterangan: * dengan proses yang sama dilakukan pada kulit jeruk jingga segar

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Lampiran 15. Kromatogram minyak atsiri kulit buah jeruk jingga segar

UNIVERSITAS SUMATERA UTARA
FAKULTAS FARMASI
LABORATORIUM PENELITIAN
Jl. Almamater No. 5 Kampus USU Medan 20155
Sampel Information

Analyzed by
Sample Type
Level #
Sampel Name
Sample ID
Vial#
:1
Method File
Org. Method File
SendlfSModified by

: Admin
: Unknown
:1
: jerukjinggasegar
: SF4S
: C:GCMSsolution Data Project1 analisajerukjingga.qgm
: C:GCMSsolution Data Project1 analisajerukjingga.qgm
: Admin

Chromatogram jerukjinggasegar C:GCMSsolution Data Project1 analisajerukjingga.qgm/jerukjinggasegar.qgd

Peak#

R.Time

Area
201631

Area%
0.46

Height

Name

1

1.691

154667

Pentane, 2-methyl-

2

1.732

244141

3

1.780

6317918

0.56

186809

Pentane, 3-methyl-

14.39

3824770

4

1.894

409184

0.93

286382

Cyclopentane, methyl-

5

6.738

406176

0.92

151986

Bicyclo[3.1.0]hex-2-ene, 2-methyl-5-1(1-methylethyl)-

6

6.963

1325895

3.02

448726

.alpha-Pinene$$Bicyclo[3.1.1]hept-2-ene,2,6,6-trimethyl-$$2-P

Hexane

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7

8.264

1165022

2.65

339742

8

8.408

4609836

10.50

1175092

.beta-Phellandrene
.beta-Pinene$$Bicyclo[3.1.1heptane,6,6-dimethyl-2-methylene-

9

8.886

145632

0.33

54274

10

8.992

985966

2.25

339526

11

9.930

264553

0.40

82647

12

10.044

525676

1.20

140969

13

10.565

17113830

38.97

1814535

Limonene

14

11.613

8404245

19.14

1627782

3-Carene$$Bicyclo[4.1.0]hept-3-ene,3,7,7-trimethyl-$$.delta(S

15

11.8673

118454

0.27

39232

16

12.716

692891

1.58

238119

17

15.872

137084

0.31

51489

trans-Sabinenehydrate$$5-Isopropyl-2-methylbicyclo[3.1.0]hexan

18

16.300

161781

0.37

58560

p-menth-1-en-8-ol$$2-(4-methyl=3=cyclohexen-1-yl)-2-propanol

19

16.938

165226

0.38

62478

4-Decene,7-methyl-, (E)- $$(4E)-7-Methyl-4decene#$$

20

26.552

110876

0.25

34400

1,3-Benzodioxole, 4-Methoxy-6-(2-propenyl)- $$Benzene,5-allyl-

21

26.898

268611

0.61

88521

.alpha.-Cubebene

22

27.862

142262

0.32

48557

1,3,6,10-Dodecatetraene,3,7,11-trimethyl-(Z,E)-

43916890

Octanal
1,4-Methano-1H-Cyclopropa(d)pyridazine,4,4a,5,5a-tetrahydro
1,4-Cyclohexadiene,1-methyl-4-(1-methylethyl)Benzene, 1-methyl-4-(1-methylethyl)-

1-Octanol
Pentane,3-bromo-$$ 3-Bromopentane$$ 3-Pentyl bromide $$

100.00 11249263

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Lampiran 16. Spektrum massa puncak dengan waktu tambat 6,958 menit

Lampiran 17. Spektrum massa puncak dengan waktu tambat 8,242 menit

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Lampiran 18. Spektrum massa puncak dengan waktu tambat 8,400 menit

Lampiran 19. Spektrum massa puncak dengan waktu tambat 10,483 menit

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Lampiran 20. Spektrum massa puncak dengan waktu tambat 11,543 menit

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Lampiran 21. Kromatogram minyak atsiri kulit buah jeruk jingga kering

UNIVERSITAS SUMATERA UTARA
FAKULTAS FARMASI
LABORATORIUM PENELITIAN
Jl. Almamater No. 5 Kampus USU Medan 20155
Sampel Information

Analyzed by
: Admin
Sample Type
: Unknown
Level #
:1
Sampel Name
: jerukjinggakering
Sample ID
: SF4S
Vial#
:1
Method File
: C:GCMSsolution Data Project1 analisajerukjingga.qgm
Org. Method File : C:GCMSsolution Data Project1 analisajerukjingga.qgm
SendlfSModified by
: Admin
Chromatogram jerukjinggakering C:GCMSsolution Data Project1 analisajerukjingga.qgm/jerukjinggakering.qgd

Peak#

R.Time

Area

Area%

Height
343641

Name

1

1.479

489903

0.93

Ethanol

2

1.691

106862

0.20

83931

3

1.780

212906

0.40

165580

4

1.894

6031988

11.46

3687313

5

6.738

403032

0.77

277252

Cyclopentane, methyl-

6

6.963

538594

1.02

199627

Bicyclo[3.1.0]hex-2-ene, 2-methyl-5-1(1-methylethyl)-.

7

8.264

1777126

3.38

587950

alpha-Pinene$$Bicyclo[3.1.1]hept-2-ene,2,6,6-trimethyl-$$2-P

8

8.408

1394415

2.65

371230

.beta-Phellandrene.

9

8.886

5647623

10.73

1267850

10

8.992

1406486

2.67

464031

Pentane, 2-methylButyl isocyanatoacetate $$ n-Butylisocyanatoacetate$$Acetic
Hexane$$n-Hexane$$SkellysolveB$$n-C6H14$$Esani$$

.beta-Pinene
.beta-Myrcene

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11

9.930

367331

0.70

100085

1,4-Cyclohexadiene,1-methyl-4-(1-methylethyl)-

12

10.044

950131

1.81

205367

Benzene, 1-methyl-4-(1-methylethyl)-

13

10.565

21929433

41.67

2071114

Limonene

14

11.613

8888940

16.89

1549605

3-Carene

15

11.8673

148044

0.28

57449

16

12.716

779246

1.48

262356

Cyclohexene, 1-methyl-4-(1-methylethylidene)- $$p-Mentha-1

17

15.872

317835

0.60

110852

trans-Sabinenehydrate$$5-Isopropyl-2-methylbicyclo[3.1.0]hexan

18

16.300

386644

0.73

135730

p-menth-1-en-8-ol$$2-(4-methyl=3=cyclohexen-1-yl)-2-propanol

19

16.938

139889

0.27

53245

Acetic acid, octyl acetate$$ n-Octyl acetate$$Capyrylyl acetate$$

20

26.552

424602

0.81

137718

1,6-Cyclodecadiene, 1-methyl-5-methylene-8-(1-methylethyl)-

21

26.898

281069

0.53

94567

.cis-.alpha-Bisabolene$$4-(1Z)-1,5-Dimethyl-1,4-hexadienyl]

22

27.862

52622099

100.00

1226493

2-Furanmethanol, 5-ethenyltetrahydro-.alpha.,alpha.,5-trimethyl

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Lampiran 22. Spektrum massa puncak dengan waktu tambat 6,975 menit

Lampiran 23. Spektrum massa puncak dengan waktu tambat 8,425 menit

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Lampiran 24. Spektrum massa puncak dengan waktu tambat 9,008 menit

Lampiran 25. Spektrum massa puncak dengan waktu tambat 10,617 menit

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Lampiran 26. Spektrum massa puncak dengan waktu tambat 11,633 menit

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Lampiran 27. Gambar pola fragmentasi komponen minyak atsiri kulit buah jeruk
jingga segar
1. α-Pinen (Rt 6,958 menit)

C10H16˥+
m/z 136
C4H2

C9H13˥+

CH4
16

C8H9˥+

m/z 121

m/z 105

C2H4
28

C6H5˥+
m/z 77

C2H3˥+
m/z 27

50
2.

CH3
15

β-phelladren (Rt 8,242 menit)

C10H16˥ +
m/z 136
C4H2

CH3
15

C9H13˥+
m/z 121

CH4
16

C8H9˥+
m/z 105

C2H4
28

C6H5˥+
m/z 77

C2H3˥+
m/z 27

50

3. β-pinen (Rt 8,400 menit)

+

C10H16˥
m/z 136
CH2
14

CH3
15
C6H7˥+
m/z 79

C9H13˥
m/z 121
+

C2H2
26

CH2
14

C4H5˥+
m/z 53

C8H11˥+
m/z 107
C2H2
26

CH2
14

C7H9˥+
m/z 93

C2H3˥+
m/z 27

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Lampiran 27 (lanjutan)
4. Limonen (Rt 10,483 menit)

C10H16˥+
m/z 136
CH2
14

CH3
15

C6H7˥+
m/z 79

C9H13˥+
m/z 121
C2H2
26

CH2
14

C4H5˥+
m/z 53

C8H11˥+
m/z 107
C2H2
26

CH2
14

C7H9˥+
m/z 93

C2H3˥+
m/z 27

5. 3-caren (Rt 11,583 menit)

C10H16˥ +
m/z 136
C3H2
38

CH3
15
C3H5˥+
m/z 41

C9H13˥+
m/z 121
CH2
14

CH4
16

C8H9˥+
m/z 105

C2H2
26

C6H7˥+
m/z 79

C2H3˥+
m/z 27

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Lampiran 28. Gambar pola fragmentasi komponen minyak atsiri kulit buah jeruk
jingga kering
1. α-pinen (Rt 6,975 menit)

CH3
C9H13˥+
15 m/z 121

C10H16˥ +
m/z 136
C4H2
50

CH4
16

C8H9˥+
m/z 105

CH2
14

C8H11˥+
m/z 107

C2H4
28

C6H5˥+
m/z 77

C2H3˥+
m/z 27

2. β-pinen (Rt 8,425 menit)

CH3
15

C10H16˥+
m/z 136
CH2
14

C6H7˥+
m/z 79

C9H13˥+
m/z 121
C2H2
26

C4H5˥+
m/z 53

C2H2
26

CH2
14

C7H9˥+
m/z 93

C2H3˥+
m/z 27

3. β-mirsen (Rt 9,008 menit)

C10H16˥ +
m/z 136
CH2

CH3
15

C9H13˥+
m/z 121
C2H2

CH2
14

C8H11˥
m/z 107

+

CH2
14

C7H9]+
m/z 93

C2H2

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C6H7˥+
C4H5˥+
14
26
m/z 79
m/z 53
Lampiran 28 (lanjutan)
4. Limonen (Rt 10,617 menit)

C10H16˥+
m/z 136
CH2
14

CH3
15

C6H7˥+
m/z 79

C9H13˥+
m/z 121
C2H2
26

CH2
14

C4H5˥+
m/z 53

26

C2H3˥+
m/z 27

C8H11˥+
m/z 107
C2H2
26

CH2
14

C7H9˥+
m/z 93

C2H3˥+
m/z 27

5. 3-caren (Rt 11,633 menit)

C10H16˥ +
m/z 136
C3H2
38

CH3
15

C3H5˥+
m/z 41

C9H13˥+
m/z 121
CH2
14

CH4
16

C8H9˥+
m/z 105

C2H2
26

C6H7˥+
m/z 79

C2H3˥+
m/z 27

.

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