Isolasi Minyak Atsiri Dari Kulit Buah Jeruk Kasturi (Citrus microcarpa Bunge) Segar Dan Kering Serta Analisis Komponennya Secara Gc-Ms

  Lampiran 1. Hasil identifikasi tumbuhan

  Lampiran 2. Gambar tumbuhan jeruk kasturi dan buah jeruk kasturi

  Tumbuhan jeruk kasturi Buah jeruk kasturi

  Buah jeruk kasturi

  Lampiran 3 . Gambar kulit buah jeruk kasturi segar dan kering serta serbuk

  simplisia kulit buah jeruk kasturi Kulit buah jeruk kasturi segar

  Kulit buah jeruk kasturi kering Serbuk simplisia kulit buah jeruk kasturi

  

Lampiran 4. Hasil pemeriksaan mikroskopik penampang melintang kulit buah

  jeruk kasturi segar (perbesaran 10x40)

  1

  2

  3

  4

  5

  6

  7 Keterangan :

  1. Kutikula

  2. Epidermis

  3. Kristal kalsium oksalat berbentuk prisma

  4. Kelenjar minyak atsiri

  5. Rongga minyak lisigen

  6. Parenkim

  7. Berkas pembuluh

  Lampiran 5. Hasil pemeriksaan mikroskopik serbuk simplisia kulit buah jeruk

  kasturi (perbesaran 10x40)

  1

  2

  4

  3 Keterangan:

  1. Parenkim

  2. Kristal kalsium oksalat bentuk prisma

  3. Berkas pembuluh

  4. Fragmen rongga minyak lisigen

  Lampiran 6. Alat –alat yang digunakan

  Alat penetapan kadar air Alat penetapan kadar minyak atsiri

  Lampiran 6. (Lanjutan)

  Alat destilasi air Alat refraktometer Abbe

  Lampiran 6. (Lanjutan)

  Alat Gas Chromatography – Mass Spectra Piknometer

  Lampiran 7. Perhitungan penetapan kadar air dari simplisia kulit buah jeruk

  7,99% Sampel III Volume I = 2,6 ml

  3

  = 7,99%+7,99%+7,99%

  7,99% Kadar air rata-rata

  =

  5,002 100%

  3,0 −2,6

  =

  Volume II = 3,0 ml Berat sampel = 5,002 g Kadar air

  =

  kasturi Kadar air = volume II

  5,001 100%

  2,6 −2,2

  =

  Sampel II Volume I = 2,2 ml Volume II = 2,6 ml Berat sampel = 5,001 g Kadar air

  = 7,99%

  5,001 100%

  2,2 −1,8

  Sampel I Volume I = 1,8 ml Volume II = 2,2 ml Berat sampel = 5,001 g Kadar air =

  −volume I berat sampel 100%

  = 7,99%

  Lampiran 8. Perhitungan penetapan kadar sari larut dalam air dari simplisia

  kulit buah jeruk kasturi Berat sari 100

  Kadar sari larut dalam air = 100%

  Berat sampel

  20 Sampel I Berat sampel = 5,000 g Berat sari = 0,211 g

  0,211 100 Kadar sari larut dalam air = 100%

  5,000

  20 21,1%

  =

  Sampel II Berat sampel = 5,000 g Berat sari = 0,228 g

  0,228 100 Kadar sari larut dalam air

  = 100%

  5,000

  20

  = 22,8%

  Sampel III Berat sampel = 5,000 g Berat sari = 0,2138 g

  0,2138 100 Kadar sari larut dalam air = 100%

  5,000

  20

  = 21,38% 21,1%+22,8%+21,38%

  Kadar sari larut dalam air rata-rata

  =

  3

  = 21,76%

  Lampiran 9. Perhitungan penetapan kadar sari larut dalam etanol dari

  simplisia kulit buah jeruk kasturi Berat sari 100

  Kadar sari yang larut dalam etanol = 100% Berat sampel

  20 Sampel I Berat sampel = 5,000 g Berat sari = 0,1829 g

  0,1829 100 Kadar sari yang larut etanol 100%

  =

  5,000

  20

  = 18,29%

  Sampel II Berat sampel = 5,000 g Berat sari = 0,1909 g

  0,1909 100 Kadar sari yang larut etanol = 100%

  5,000

  20 19,09%

  =

  Sampel III Berat sampel = 5,000 g Berat sari = 0,1908 g

  0,1908 100 Kadar sari yang larut etanol

  = 100%

  5,000

  20 19,08%

  = 18,29%+19,09%+19,08%

  Kadar sari larut dalam etanol rata =

  3

  = 18,82%

  Lampiran 10. Perhitungan penetapan kadar abu total dari simplisia kulit buah

  =

  3

  = 5,5417 %+5,4473%+5,5472%

  Kadar abu total rata-rata

  = 5,5472%

  100%

  0,111 2,001

  =

  Berat abu = 0,111 g Kadar abu

  5,4473% Sampel III Berat sampel = 2,001 g

  100%

  jeruk kasturi Kadar abu =

  0,109 2,001

  =

  Berat abu = 0,109 g Kadar abu

  5,5417% Sampel II Berat sampel = 2,0001 g

  =

  100%

  0,111 2,003

  Berat abu = 0,111 g Kadar abu =

  100 % Sampel I Berat sampel = 2,003 g

  Berat abu Berat sampel

  = 5,51%

  Lampiran 11. Perhitungan penetapan kadar abu tidak larut dalam asam dari

  =

  3

  = 0,3395%+0,3498%+0,3648%

  Kadar abu tidak larut dalam asam rata-rata

  = 0,3648%

  100%

  0,0073 2,001

  =

  Berat abu = 0,0073 g Kadar abu

  0,3498% Sampel III Berat sampel = 2,001 g

  100%

  simplisia kulit buah jeruk kasturi Kadar abu tidak larut dalam asam =

  0,0071 2,001

  =

  Berat abu = 0,0071 g Kadar abu

  0,3395% Sampel II Berat sampel = 2,001 g

  =

  100%

  0,0068 2,003

  Berat abu = 0,0068 g Kadar abu =

  100% Sampel I Berat sampel = 2,003 g

  Berat Abu Berat Sampel

  = 0,35%

  Lampiran 12. Penetapan kadar minyak atsiri kulit buah jeruk kasturi segar

  Volume minyak atsiri Kadar minyak atsiri =

  100% Berat sampel

  Sampel I Volume minyak atsiri = 0,14 ml Berat sampel = 15,025 g

  0,14 Kadar minyak atsiri =

  100% 15,025

  = 0,9318% Sampel II

  Volume minyak atsiri = 0,14 ml Berat sampel = 15,020 g

  0,14 Kadar minyak atsiri =

  100% 15,020

  = 0,9321% Sampel III

  Volume minyak atsiri = 0,14 ml Berat sampel = 15,025 g

  0,14 Kadar minyak atsiri =

  100% 15,025

  = 0,9318%

  0,9318%+0,9321%+0,9318%

  Kadar minyak atsiri rata-rata

  =

  3

  = 0,93%

  Lampiran 13. Penetapan kadar minyak atsiri kulit buah jeruk kasturi kering

  Volume minyak atsiri Kadar minyak atsiri =

  100% Berat sampel

  Sampel I Volume minyak atsiri = 0,19 ml Berat sampel = 15,022 g

  0,19 Kadar minyak atsiri =

  100% 15,022

  = 1,2648% Sampel II

  Volume minyak atsiri = 0,19 ml Berat sampel = 15,020 g

  0,19 Kadar minyak atsiri =

  100% 15,020

  = 1,2650% Sampel III

  Volume minyak atsiri = 0,19 ml Berat sampel = 15,022 g

  0,19 Kadar minyak atsiri =

  100% 15,022

  = 1,2648%

  1,2648%+1,2650%+1,2648%

  Kadar minyak atsiri rata-rata

  =

  3

  = 1,27%

  Lampiran 14. Penetapan indeks bias minyak atsiri kulit buah jeruk kasturi segar

  Sampel I = 1,4240 Sampel II = 1,4240 Sampel III = 1,4240

  1,4240 +1,4240+1,4240

  Indeks bias rata-rata =

  3

  = 1,4240

  Lampiran 15. Penetapan indeks bias minyak atsiri kulit buah jeruk kasturi kering

  Sampel I = 1,4240 Sampel II = 1,4240 Sampel III = 1,4240

  1,4240 +1,4240+1,4240

  Indeks bias rata-rata =

  3

  = 1,4240

  Lampiran 16. Penetapan bobot jenis minyak atsiri kulit buah jeruk kasturi segar

  Sampel III Bobot piknometer kosong = 6,5415 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2465 Bobot jenis minyak atsiri

  3

  0,8527 +0,8526+0,8524

  0,8524 Bobot jenis rata-rata =

  =

  8,5418 −6,5415

  8,2465 −6,5415

  =

  = 0,8526

  Sampel I Bobot piknometer kosong = 6,5415 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2472 Bobot jenis minyak atsiri

  8,5418 −6,5415

  8,2470 −6,5415

  Sampel II Bobot piknometer kosong = 6,5415 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2470 Bobot jenis minyak atsiri =

  = 0,8527

  8,5418 −6,5415

  8,2472 −6,5415

  =

  = 0,8526

  Lampiran 17. Penetapan bobot jenis minyak atsiri kulit buah jeruk kasturi kering

  Bobot piknometer kosong = 6,5414 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2464 Bobot jenis minyak atsiri

  3

  0,8522 +0,8521+0,8523

  Bobot jenis rata-rata =

  = 0,8523

  8,5418 −6,5415

  8,2464 −6,5414

  =

  0,8521 Sampel III

  Sampel I Bobot piknometer kosong = 6,5415 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2461 Bobot jenis minyak atsiri

  =

  8,5418 −6,5415

  8,2460 −6,5415

  Sampel II Bobot piknometer kosong = 6,5415 Bobot piknometer + air suling = 8,5418 Bobot piknometer + minyak atsiri = 8,2460 Bobot jenis minyak atsiri =

  = 0,8522

  8,5418 −6,5415

  8,2461 −6,5415

  =

  = 0,8522

  Penetapan Kadar Minyak Atsiri*

  3. PK Abu

  Bobot Jenis Minyak Atsiri dan Air

  Indeks Bias Spektrum MS Kromatogram GC

  dengan GC-MS Secara Fisika Secara Fisikokimia

  2 O

  x H

  4

  2 SO

  Minyak atsiri Na

  4. PK Sari

  2. PK Air

  1. Mikroskopis

  Minyak atsiri dengan kemungkinan adanya air Air

  Serbuk Simplisia Isolasi Minyak Atsiri dikarakterisasi

  Simplisia dihaluskan didestilasi air *

  Kulit Buah Jeruk Kasturi dibersihkan dikeringkan

  (Citrus microcarpa Bunge)

  Lampiran 18. Flowsheet isolasi minyak atsiri kulit buah jeruk kasturi

• Larut air
• Larut etanol
• Catatan: dengan cara yang sama dilakukan dengan kulit buah jeruk kasturi yang telah dikeringkan.

  diidentifikasi

  2 SO 4 anhidrat

  dipisahkan ditambah Na

• Total • Tidak Larut Asam

  Lampiran 19. Kromatogram GC minyak atsiri kulit buah jeruk kasturi segar UNIVERSITAS SUMATERA UTARA

FAKULTAS FARMASI

LABORATORIUM PENELITIAN

  JL. Almamater No. 5 Kampus USU Medan 20155 Peak# R.Time Area Area% Peak Report Height TIC

  Name 1 1.595 8575428 9.22 3344802 Hexane 2 1.712 186687 0.20 134045 Cyclopentane, methyl- $$ Methylcyclopentan 3 6.565 1532857 1.65 404414 .alpha.-Pinene 4 8.024 344213 0.37 91823 Cyclohexene, 4-methylene-1-(1-methylethyl) 5 8.142 1072522 1.15 239957 .beta.-Pinene 6 8.721 5822725 6.26 865527 .beta.-Myrcene 7 10.681 71641135

  77.03 2642655 Limonene 8 11.924 103466 0.11 39133 1-Octanol 9 12.607 24830 0.03 9548 2-Cyclopenten-1-one, 2,3,5-trimethyl-4-meth 10 13.059 331353 0.36 112310 1,6-Octadien-3-ol, 3,7-dimethyl- 11 13.239 174132 0.19 61416 Nonanal 12 13.725 10180 0.01 4168 1-Propanone, 1-cyclopropyl- 13 15.887 12686 0.01 7833 1-Hexanol, 3-methyl- 14 16.103 34294 0.04 12893 3-Methyl-hepta-1,6-dien-3-ol $$ 3-Methyl-1, 15 16.620 87619 0.09 30821 3-Cyclohexene-1-methanol, .alpha.,.alpha.4-t 16 17.187 299857 0.32 89852 Decanal 17 17.430 25281 0.03 11093 1-Octene 18 19.269 12759 0.01 5727 Methyl vinyl ketone 19 20.921 26269 0.03 10622 Hexanal 20 22.938 33512 0.04 11439 1-Penten-3-one, 2,4-dimethyl- $$ 2,4-Dimeth 21 23.598 523469 0.56 146201 2,6-Octadien-1-ol, 3,7-dimethyl-, acetate, (E) 22 24.430 32564 0.04 9242 Propane, 1-bromo-2-methyl- 23 26.920 1850203 1.99 426555 1,6-Cyclodecadiene, 1-methyl-5-methylene-8 24 31.575 92698

  0.10 27915 Naphthalene, hexahydro-1,6-dimethyl-4- 25 32.137 153510 0.17 44517 2-Naphthalenemethanol, 2,3,4,4a,5,6,7,8- 93004249 100.00 8784508

  Lampiran 20. Pola fragmentasi komponen minyak atsiri kulit buah jeruk kasturi

  segar 1. α-pinen dengan waktu retensi 6,567 menit ⁺ • CH ^{3 C 2 H 4}

  C H H m/z 121 C H m/z 93

  10 16  m/z 136 C

  9 13 

  7 9 

• 28
• 15 C
^{2 H 2} C ^{2 H} 2<
• +

  C

  5 H 7 m/z 67 C

  3 H 5 m/z 41

   

• 26 -26 2.

  β-pinen dengan waktu retensi 8,142 menit

• ₃

  CH ²

• CH
• C

  16

• 10 H

  9 H 13 m/z 121 C

  8 H 11 m/z 107

   m/z 136 C  

• 14
• 15 CH
² CH C + + ^{2 + 2 H 2} C

  7 H 9  m/z 93 C

  6 H 7  m/z 79 C

  4 H 5  m/z 53

• 26
14 C + ^{2 H 2} C H m/z 27

  2 3 

• 26

  Lampiran 20. (lanjutan) 3.

  β-mirsen dengan waktu retensi 8,725 menit

• CH
3<

  CH ²

• C

  10 H 16  m/z 136 C

  9 H 13 

  m/z 121 C

  8 H 11  m/z 107

• 15 -14 CH
² C ^{2 H 2} CH 2<
• + +

  C H m/z 93 C H m/z 79

  7 9 

  6 7 

• 14
26 C
• ^{+ 2 H}
² + C

  4 H 5 m/z 53 C

  2 H 3 m/z 27

   

• 26

  4. Limonen dengan waktu retensi 10,683 menit

• CH
^{3 +} CH 2<
• C H C H m/z 121 C H m/z 107

  10 16  m/z 136

  9 13  8 

  11

• 14
• 15

  C ^{2 H 2} CH ² CH ²

• +

  C

  7 H 9  m/z 93 C

  6 H 7 

  m/z 79

• 14
14 C ^{2 H} 2<

  C

  4 H 5 m/z 53 C

  2 H 3 m/z 27

   

• 26

  Lampiran 20. (lanjutan)

  5. Geranil asetat dengan waktu retensi 23,600 menit _{O O}

• _{+ +}
• C
^{2 H 2 O} H 2 O<

  C

  12 H

  20 O 2  m/z 196 C

  10 H

  18 O  m/z 154 C

  10 H 16  m/z 136

• 18
• 42

  CH ²

• CH
₃ CH 2<

• + + +

  C H m/z 121 C H m/z 107 C H m/z 93

  9 13 

  8

11 

  7 9 

• 15
14 CH

  C ^{3 H 3 CH 2}

• + +

  C H m/z 80 C H m/z 41 C H m/z 27

  6 8 

  3

5 

  2 3 

• 39

  13

• 14

  6. Germakren dengan waktu retensi 26,917 menit ₊ •C CH _{3 H 7} ²

  C H

  15 m/z 204 C 24 

  12 H 17  m/z 161 C

  15  m/z 147

• 11 H
• 14
• 43 CH
^{2 CH 2 CH} 2<
• + +

  C

  10 H 13  m/z 133 C

  9 H 11  m/z 119

• 14
14 C ^{4 H 2} CH 2<

  C H m/z 105 C H m/z 91 C H m/z 41

  8 9 

  7 7 

  3 5 

• 14

  50 CH ² + C

  2 H 3 m/z 27

  

• 14

  Lampiran 21. Kromatogram GC minyak atsiri kulit buah jeruk kasturi kering

UNIVERSITAS SUMATERA UTARA

FAKULTAS FARMASI

LABORATORIUM PENELITIAN

  JL. Almamater No. 5 Kampus USU Medan 20155 Peak# R.Time Area Area% Peak Report

  Height TIC

  0.06 19759 3-Cyclohexene-1-methanol, l h l h 4 t 12 17.021 14116

  0.24 76880 Styrene 3 6.596 1838577

  2.05 510339 .alpha.-Pinene 4 8.056 304356

  0.34 89319 .beta.-Phellandrene 5 8.172 1009252

  1.13 249509 .beta.-Pinene 6 8.751 5837317

  6.51 999217 .beta.-Myrcene 7 10.671 68171524

  76.02 2604738 Limonene 8 13.080 300342

  0.33 103936 1,6-Octadien-3-ol, 3,7-dimethyl- 9 13.262 60440

  0.07 24097 Decanal 10 16.122 21470

  0.02 8219 Pentane, 3-bromo- 11 16.639 51140

  0.02 5542 1-Hexene, 3,4-dimethyl- 13 17.204 120215

  TIC Name 1 1.597 9798974

  0.13 43018 Dodecanal 14 17.448 45033

  0.05 18126 Acetic acid, octyl ester $$ n-Octyl acetate $$ 15 18.661 23293

  0.03 8586 2-Cyclohexen-1-one, 2-methyl-5-(1- th l t 16 22.041 58324

  0.07 18005 Cyclohexene, 3-methyl-6-(1- th l th lid 17 22.949 31126

  0.03 10505 1-Penten-3-one, 2,4-dimethyl- $$ 2,4- Di th 18 23.608 397824

  0.44 109219 2,6-Octadien-1-ol, 3,7-dimethyl-, acetate, (E) 19 26.925 1350886

  1.51 323162 1,6-Cyclodecadiene, 1-methyl-5- th l

  8 20 27.432 30519 0.03 11189 1,5-Heptadiene, 2,5-dimethyl-3-methylene-

  $ 89675554

  10.93 3569301 Hexane 2 5.183 210826

  Peak Report Height

  Name 1 1.597 9798974 10.93 3569301 Hexane

  0.02 8219 Pentane, 3-bromo- 11 16.639 51140

  2 5.183 210826

  0.24 76880 Styrene 3 6.596 1838577

  2.05 510339 .alpha.-Pinene 4 8.056 304356

  0.34 89319 .beta.-Phellandrene 5 8.172 1009252

  1.13 249509 .beta.-Pinene 6 8.751 5837317

  6.51 999217 .beta.-Myrcene 7 10.671 68171524

  76.02 2604738 Limonene 8 13.080 300342

  0.33 103936 1,6-Octadien-3-ol, 3,7-dimethyl- 9 13.262 60440

  0.07 24097 Decanal 10 16.122 21470

  0.06 19759 3-Cyclohexene-1-methanol, l h l h 4 t 12 17.021 14116

  100.00 8802666 Peak# R.Time Area Area%

  0.02 5542 1-Hexene, 3,4-dimethyl- 13 17.204 120215

  0.13 43018 Dodecanal 14 17.448 45033

  0.05 18126 Acetic acid, octyl ester $$ n-Octyl acetate $$ 15 18.661 23293

  0.03 8586 2-Cyclohexen-1-one, 2-methyl-5-(1- th l t 16 22.041 58324

  0.07 18005 Cyclohexene, 3-methyl-6-(1- th l th lid 17 22.949 31126

  0.03 10505 1-Penten-3-one, 2,4-dimethyl- $$ 2,4- Di th 18 23.608 397824

  0.44 109219 2,6-Octadien-1-ol, 3,7-dimethyl-, acetate, (E) 19 26.925 1350886

  1.51 323162 1,6-Cyclodecadiene, 1-methyl-5- th l

  8 20 27.432 30519 0.03 11189 1,5-Heptadiene, 2,5-dimethyl-3-methylene-

  $ 89675554

  100.00 8802666

  Lampiran 22. Pola fragmentasi komponen minyak atsiri kulit buah jeruk kasturi

  kering 1. α-pinen dengan waktu retensi 6,600 menit

• CH
^{3 C 2 H 4}

  C

  10 H 16  m/z 136 C

  9 H 13  m/z 121 C

  7 H 9 

  m/z 93

• 28
• 15 C
^{2 H 2} C ² H + + ² C

  5 H 7  m/z 67 C

  3 H 5  m/z 41

• 26 -26 2.

  β-pinen dengan waktu retensi 8,142 menit

  CH ^{2 +} • CH ³ C

  9 13  m/z 121 C

  8 H 11  m/z 107

  10 H 16  m/z 136 C H •

• 14
• 15 CH
² CH

^{2 C}

+ ^{+ 2 H + 2} C

  7 H 9  m/z 93 C

  6 H 7  m/z 79 C

  4 H 5  m/z 53

• 26
14 C + ^{2 H 2} C H m/z 27

  2 3 

• 26

  Lampiran 22. (lanjutan) 3.

  β-mirsen dengan waktu retensi 8,750 menit

• CH
3<

  CH ²

• C

  10 H 16  m/z 136 C

  9 H 13 

  m/z 121 C

  8 H 11  m/z 107

• 15 -14 CH
² C ^{2 H 2} CH 2<
• + +

  C H m/z 93 C H m/z 79

  7 9 

  6 7 

• 14
26 C H + + ^{2 2} C

  4 H 5 m/z 53 C

  2 H 3 m/z 27

   

• 26

  4. Limonen dengan waktu retensi 10,675 menit ⁺ •CH ³ CH ²

• 10

  C H C H m/z 121 C H m/z 107

  16  m/z 136

  9 13 

  8 11 

• 14
• 15

  CH ² C ^{2 H 2} CH ²

• +

  C H m/z 93 C H m/z 79

  7 9 

  6 7 

• 14
14 C ^{2 H} 2<

  C

  4 H 5 m/z 53 C

   

  2 H 3 m/z 27

• 26

  Lampiran 22. (lanjutan)

  5. Geranil asetat dengan waktu retensi 23,608 menit _{O O}

• _{+ +}
• C
^{2 H 2 O} H 2 O<
• C

  12 H

  20 O 2  m/z 196 C

  10 H

  18 O  m/z 154 C

  10 H 16  m/z 136

• 18
• 42

  CH ²

• CH
³ CH 2<

• + + +

  C H m/z 121 C H m/z 107 C H m/z 93

  9 13 

  8

11 

  7 9 

• 15
14 CH

  C ^{3 H 3 CH 2}

• + +

  C H m/z 80 C H m/z 41 C H m/z 27

  6 8 

  3

5 

  2 3 

• 39

  13

• 14

  6. Germakren dengan waktu retensi 26,925 menit

• C
_{3 H 7 CH 2}
• ⁺ +
• C H

  15 m/z 204 C 24 

  12 H 17  m/z 161 C

  15  m/z 147

• 11 H
• 14
• 43 CH
^{2 CH 2 CH} 2<
• + +

  C

  10 H 13  m/z 133 C

  9 H 11  m/z 119

• 14
14

  C ^{4 H 2} CH ²

  C H m/z 105 C H m/z 91 C H m/z 41

  8 9 

  7 7 

  3 5 

• 14

  50 CH ²

• C H

  m/z 27

  2 3 

• 14