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

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Lampiran 2. Gambar tumbuhan jeruk jingga dan buah jeruk jingga

A

a

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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

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Lampiran 4. Alat–alat yang digunakan

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Gambar alat penetapan kadar minyak atsiri

Lampiran 4. (Lanjutan)

Gambar alat destilasi air

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Lampiran 4. (Lanjutan)

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Gambar Gas Chromatograph– Mass Spectrometer

Lampiran 5. Hasil pemeriksaan mikroskopik serbuk simplisia kulit buah jeruk jingga (perbesaran 10x40)

Keterangan :

1. Fragmen

rongga minyak skizolisigen

2. Parenkim

dengan kristal kalsium oksalat bentuk prisma

3. Berkas

pembuluh 4. Parenkim

2

3 1

(8)

Lampiran 6. Penetapan kadar air

a. Berat sampel = 5,0090 g Volume I = 0,1 ml

Volume II = 0,5 ml

Kadar air =

=

7,98%

b. Berat sampel = 5,0080 g Volume I = 0,5 ml Volume II = 0,9 ml

Kadar air = x 100%

=

7,98%

c. Berat sampel = 5,0020 g Volume I = 0,9 ml

Volume II = 1,3 ml

Kadar air

=

x 100%

=

7,99%

Kadar air rata-rata =

(9)

Lampiran 7. Penetapan kadar sari yang larut dalam air

a. Berat sampel = 5,0020 g Berat sari = 0,2017 g

Kadar sari = 100% = 20,16%

b. Berat sampel = 5,0020 g Berat sari = 0,2028 g

Kadar sari = 100% = 20,27% c. Berat sampel = 5,0020 g

Berat sari = 0,2004

Kadar sari = 100% = 20,03%

(10)

Lampiran 8. Penetapan kadar sari yang larut dalam etanol

a. Berat sampel = 5,0080 g Berat sari = 0,1116 g

Kadar sari = 100% =10,04%

b. Berat sampel = 5,0010g Berat sari = 0,1079 g

Kadar sari = 100% = 10,79%

c. Berat sampel = 5,0010 g Berat sari = 0, 1081 g

Kadar sari = 100% = 10,81%

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Lampiran 9. Penetapan kadar abu total

a. Berat sampel = 2,0090 g Berat abu = 0,075 g

Kadar abu = 100 % = 3,73 % b. Berat sampel = 2,0000 g

Berat abu = 0,0728 g

Kadar abu = 100% = 3,64%

c. Berat sampel = 2,0002 g Berat abu = 0,0725 g

Kadar abu = 100% = 3,62%

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

=

x

100%

Sampel I 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

=

(13)

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

= 4,18%

(14)

= 4,17%

b. Kadar minyak atsiri kulit buah jeruk jingga kering

Kadar minyak atsiri =

Sampel I

= 7,98 %

Sampel II

= 7,98 %

Sampel III

(15)

= 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 =

(16)

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

Sampel III

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

Bobot jenis minyak atsiri =

= 0,8529

Sampel II

Bobot piknometer kosong = 8,5415 Bobotpiknometer + air suling = 10,5418 Bobot piknometer + minyak atsiri = 10,2470

= 0,8526

Sampel III

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dipisahkan

di tambah Na2SO4 anhidrat

di identifikasi

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

Minyak atsiri dengan kemungkinan adanya air

Air 1. Mikroskopis

2. PK Air 5. PK Minyak Atsiri

Minyak atsiri Na2SO4 x H2O

dengan GC-MS Secara Fisika Secara Fisikokimia

Indeks Bias Spektrum

MS Kromatogram

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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 : Admin

Sample Type : Unknown Level # : 1

Sampel Name : jerukjinggasegar 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 jerukjinggasegar C:GCMSsolution Data Project1 analisajerukjingga.qgm/jerukjinggasegar.qgd

Peak# R.Time Area Area% Height Name

1 1.691 201631 0.46 154667 Pentane, 2-methyl- 2 1.732 244141 0.56 186809 Pentane, 3-methyl- 3 1.780 6317918 14.39 3824770 Hexane

4 1.894 409184 0.93 286382 Cyclopentane, methyl-

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7 8.264 1165022 2.65 339742 .beta-Phellandrene

8 8.408 4609836 10.50 1175092 .beta-Pinene$$Bicyclo[3.1.1heptane,6,6-dimethyl-2-methylene- 9

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

3-Carene$$Bicyclo[4.1.0]hept-3-ene,3,7,7-trimethyl-$$.delta(S 1-Octanol

Pentane,3-bromo-$$ 3-Bromopentane$$ 3-Pentyl bromide $$ trans-Sabinenehydrate$$5-Isopropyl-2-methylbicyclo[3.1.0]hexan p-menth-1-en-8-ol$$2-(4-methyl=3=cyclohexen-1-yl)-2-propanol 4-Decene,7-methyl-, (E)- $$(4E)-7-Methyl-4decene#$$ 1,3-Benzodioxole, 4-Methoxy-6-(2-propenyl)- $$Benzene,5-allyl- .alpha.-Cubebene

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Lampiran 16. Spektrum massa puncak dengan waktu tambat 6,958 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 Name 1 1.479 489903 0.93 343641 Ethanol

2 1.691 106862 0.20 83931 Pentane, 2-methyl-

3 1.780 212906 0.40 165580 Butyl isocyanatoacetate $$ n-Butylisocyanatoacetate$$Acetic 4 1.894 6031988 11.46 3687313 Hexane$$n-Hexane$$SkellysolveB$$n-C6H14$$Esani$$ 5 6.738 403032 0.77 277252 Cyclopentane, methyl-

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

Limonene 3-Carene

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Lampiran 27. Gambar pola fragmentasi komponen minyak atsiri kulit buah jeruk jingga segar

1. α-Pinen (Rt 6,958 menit)

2. β-phelladren (Rt 8,242 menit)

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Lampiran 27 (lanjutan)

4. Limonen (Rt 10,483 menit)

C10H16˥ C9H13˥+ C8H11˥+ C7H9˥+

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

(31)

Lampiran 28. Gambar pola fragmentasi komponen minyak atsiri kulit buah jeruk jingga kering

(32)

C6H7˥+ C4H5˥+ C2H3˥+ m/z 79 m/z 53 m/z 27

Lampiran 28 (lanjutan)

4. Limonen (Rt 10,617 menit)

C10H16˥ C9H13˥+ C8H11˥+ C7H9˥+

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