SNI 01-6684-2002
Standar Nasion Nasion al Indonesia
Minuman in uman energi energi
ICS 27.180
Badan Standardis Standardis asi Nasion Nasion al
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SNI 01-6684-2002
Daftar Daftar is i Hal Daftar isi ......................................................................................................................i Prakata Prakat a .......................... .............................. ............................. .............................. ..... ii 1
Ruang lingkup lingk up ............................. ............................. .............................. ............. 1
2
Acuan normatif ............... ...................... ............... ............... ............... ............... ............... ............... ............... ............... ............... ................ ........... ... 1
3
Istilah Istil ah dan definisi defini si ............................ .............................. ............................. ........ 1
4
Persyaratan Persya ratan ........................... .............................. ............................. ................... 2
5
Pengambilan Pengamb ilan contoh .............................. ............................. .............................. .. 2
6
Cara uji ............................. ............................. .............................. ........................ 2
7
Penandaan Penanda an ............................ .............................. ............................. ................... 4
8
Pengemasan Pengema san .......................... ............................. .............................. .................. 4
Lampiran Lampir an A : Taurin ............................ ............................. .............................. ............. 5 Lampiran Lampir an B : Kafein Kafei n ............................ ............................. .............................. ............. 3 Lampiran Lampir an C : Pemanis Buatan ..................................... .............................. ................ 10
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SNI 01-6684-2002
Prakata
STANDAR Nasional Indonesia (SNI) Minuman energi merupakan standar baru. Standar ini disiapkan oleh tim dari BBIHP (Balai Besar Industri Hasil Pertanian) serta Panitia Teknis Makanan dan Minuman, Departemen Perindustrian dan Perdagangan. Maksud dan tujuan penyusunan standar ini adalah sebagai acuan sehingga minuman
energi yang beredar di pasaran dapat terjarnin mutunya. Tim di atas dalam menyusun rumusan SNI telah memperhatikan hal-hal yang tertera dalam : 1.
Undang-Undang RI No. 7 tanun 1996 tentang Pangan.
2.
Undang-Undang RI No. 8 tahun 1996 tentang Perlindungan Konsumen.
3.
Peraturan Pemerintah No. 69 tahun 1999 tentang Label dan Iklan Pangan.
4.
Kumpulan Peraturan Perundang-undangan di Bidaing Makanan Edisi III Jilid I
Tahun 1993-1994. Dit. Jen POM, Dep. Kes. RI. Standar ini telah dibahas rnelalui rapat-rapat teknis di Bogor, rapat prakonsensus di Bogor pada tanggal 14 Agustus 2001 dan terakhir dibahas dalam Rapat Konsensus Nasional pada tanggal 15 Nope:nber 2001 di Jakarta. Hadir dalam rapat tersebut wakilwakil dari konsumen, produsen, lembaga ilmu pengetahuan dan teknologi, dan instansi terkait lainnya.
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SNI 01-6684-2002
Minuman energi
1
Ruang Ruang lingk up
Standar ini menetapkan acuan, definisi, persyaratan, pengambilan contoh, cara uji, penandaan dan pengemasan untuk minuman energi.
2
Acuan normatif
SNI 01-2891-1992, Cara uji makanan dan minuman SNI 01-2892-1992, Cara uji gula SNI 01-2893-1992, Cara uji pemanis buatan. SNI 01-2894-1992, Cara uji bahan pengawet makanan dan bahan tambahan yang dilarang
untuk makanan. SNI 01-2895-1992, Cara uji pewarna tambahan makanan SNI 01-2896-1998, Cara uji cemaran logam dalam makanan SNI 01-2897-1992, Cara uji cemaran mikroba SNI 01-4866-1998, Cara uji cemaran arsen dalam makanan SNI 19-0428-1998, Petunjuk pengambilan contoh padatan SNI 01-0222-1995, Bahan tambahan makanan.
Official Methods of Analysis of AOAC International, 1999, VoI.l!. 16th .ed., 5th revision, ACAC Interna I nternational tional,, Maryland Ma ryland USA.
3
Istilah dan definisi
minuman energi
minuman yang mengandung satu atau lebih bahan yang rnudah dan cepat diserap oleh tubuh untuk menghasilkan energi dengan atau tanpa bahan tambahan makanan yang diizinkan CATATAN Minuman energi bukan dimaksudkan sebagai suplemen makanan.
4
Persyaratan
Persyaratan minuman energi seperti Tabel 1 dibawah ini :
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SNI 01-6684-2002
Tabel Tabel I Persyaratan minu man energi
5
Pengambilan Pengambilan contoh
Cara pengambilan contoh sesuai dengan SNI 19-0428-1993, Petunjuk pengambilan
contoh padatan.
6
Cara Cara uji
6.1 6.1 Persi Persi apan conto h a)
Persiapan contoh sesuai dengan SNI 01-2891-1992, Cara uji makanan dan minuman
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SNI 01-6684-2002
6.2
Keadaan
Cara uji keadaan sesuai dengan SNI 01-2891-1992, Cara uji makanan dan minuman. butir 1.2. 6.3
pH
Cara uji pH sesuai dengan SNI 01-2891-1992, Cara uji makanan dan minuman butir 16. 6.4
Total energi
6.4.1
Prinsip
Total energi adalah penjumlahan dari (4 x % karbohidrat + 4 x % protein + 9 x % lemak). 6.4.2 a)
Prosedur
Tentukan air dalam contoh; SNI 01-2891-1992, Cara uji makanan dan minuman butir 5.1.
b)
Tentukan abu dalam contoh, SNI SNI 01-2891-1992, 01-2891-1992, Cara uji makanan dan minuman butir 6.1.
c)
Tentukan protein dalam contoh; SNI 01-2891-1992, Cara uji makanan dan minuman butir 7.1.
d)
Tentukan karbohidrat dalam contoh dengan cara pengurangan yaitu {100 % - (% air + % abu + % protein + % lemak)}.
6.4.3
Perhitungan
Nilai energi = ( 4 x % karbohidrat ) + ( 4 x % protein ) f- (9 x % lemak ) Kkal/100 g
= 4 (% karbohidrat + % protein) + 0 = 4 (% karbohidrat + % protein).
6.5 6.5
Total gula (dihitu ng sebagai sakarosa)
Cara uji gula (sakarosa) sesuai dengan SNI 01-2892-1992, Cara uji gula butir 3.1.
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SNI 01-6684-2002
6.9.1
Pemanis buatan
Cara uji pemanis buatan sesuai dengan SNI 01-2893--1992, Cam Uji Pemanis Buatan. a.
Jika sakarin positif, teruskan ke AOAC Official Method 934.04 - 1999. ( Lampiran C.1)
b.
Jika siklamat positif, teruskan ke AOAC Official Method 957.10 - 1999. ( Lampiran C.2)
c.
Sorbitol sesuai dengan AOAC Official Method 973.28 - 1999. ( Lampiran C.3)
6.9.2
Pengawet
Cara uji pengawet sesuai dengan SNI 01-2894-1992, Cara uji bahan pengawet makanan
dan bahan tambahan yang dilarang untuk makanan. 6.9.3
Pewarna tambahan
Cara uji pewarna tambahan sesuai dengan SNI 01-2895-1992, Cara uji pewarna
tambahan makanan. 6.10 Cemaran logam Cara uji cemaran Iogam sesuai dengan SNI 01-2896-1998, Cara uji cemaran logam dalam
makanan 6.11 Cemaran arsen Cara uji cemaran arsen sesuai dengan SNI 01-4866-1998, Cara uji cemaran arsen dalam
makanan. 6.12 Cemaran mikroba Cara uji cemaran mikroba sesuai dengan SNI 01-2897-1992, Cara uji cemaran mikroba.
7
Penandaan
Penandaan dan pelabelan sesuai dengan, undang-undang RI No.7 tahun 1996 tentang
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SNI 01-6684-2002
Lampiran A Taurin A.1 A. 1 Acu A cu an AOAC Official Method 997.05 – 1999 Taurin in Powdered Milk and Powdered Infant
Formula. A.2 A. 2 Prin Pr in si p Contoh diencerkan dengan air, protein dan lemak dipisahkan dengan cara pengendapan. Cairan diperlakukan dengan dansil klorida untuk membentuk turunan taurin, yang dipisahkan dan diidentifikasi dengan HPLC dengan detektor UV atau fluoresen. A.3 A. 3 Peralat Per alat an a)
HPLC dengan atau tanpa integrator atau PC pengolah data
Detektor : UV, panjang gelombang 254 nm dan atau Fluoresen, eksitasi 330 rim, emisi 530 nm. Kecepatan alir : 1 - 2 ml/menit Waktu elusi dansiI klorida : 10 – 15 menit (kandungan asetonitril pada fasa gerak dapat sedikit divariasi untuk menyesuaikan retensi tergantung kepada sifat khas dari kolom yang digunakan. b)
Kolom : Reversed phase basa silikat C 18 dengan ukuran 5 µm yang rekomendasikan mengandung karbon > 10%. Kolom terbuat dari stainless dan ujung kolom bertutup atau tanpa tutup. Pelindung kolom mengandung isi yang sama dengan kolom
c)
Penyaring : hidropilik membran 0,45 µm dan kertas saring medium (Whatman # 2 atau setara).
d)
Alat-alat gelas
-
Pipet atau pipet automatik;
− −
Labu ukur: 50, 100 dan 1000 ml ; Gelas ukur ;
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SNI 01-6684-2002
e)
Fasa gerak : bufer natrium asetat – asetonitril (84 16) v/v. Campur 340 ml bufer natrium asetat dan 160) ml asetonitril, saring dan hilangkan gasnya.
f)
Fasa pembersihan kolom. Setiap akan digunakan asetonitril disaring dan dihilangkan gasnya terlebih dahulu.
g)
Bufer natrium karbonat 80 mM, pH 9,5. Timbang 0,424 g natrium karbonat anhidrat ke dalam 50 ml tabu ukur dan larutkan dengan sedikit air suling dan atur pH sampai 9,5 dengan 1 M HCI dan encerkan dengan air suling sampai tanda garis. Bufer ini stabil sampai 3 bulan pada suhu kamar.
h)
Pereaksi Carrez 1. Timbang 15,0 g kalium heksasionaferat (II) anhidrat (K 4{Fe (CN)6}.3H20) ke dalam labu ukur 100 ml dan larutkan dengan air suling, encerkan sampai tanda garis. Pereaksi ini stabil sampai 3 bulan pada suhu kamar.
i)
Pereaksi Carrez 2 Timbang 30,0 g sang asetat dihidrat Zn(OAc) 2.2H20 kedalam labu ukur 100 ml dan larutkan dengan air suling. Encerkan sampai tanda cair. Pereaksi ini stabil sampai 3 bulan pada suhu kamar.
j)
Pereaksi dansil klorida 1,5 mg/ml Larutkan 15 mg, 5 dimetil aminonaftalen – 1 – sulfonil kiorida (dansil klorida) dalam 10 ml asetonitril. Pereaksi ini disiapkan tiap hari (baru).
k)
Larutan metilamin hidroklorida 20' mg/ml. Larutkan 2,0 g metilamin hidroklorida dalam 100 ml air suling. Cara lain : encerkan 2,0 ml larutan encer 25% rnenjadi 25 ml. Larutan ini stabil sampai 3 bulan pada suhu 4°C.
I)
Larutan standar taurin
–
Larutan baku standar st andar taurin 0,1 0, 1 mg/ml. Timbang dengan teliti kira-kira 10 mg taurin dan larutkan dalam 100 ml air suling. Larutan ini stabil sampai 1 minggu pada suhu 4°C.
–
Larutan deret standar s tandar taurin. Larutkan larutan baku standar taurin dengan air suling sehingga diperoleh larutan dengan kepekatan 5; 10, 15; dan 20 µg/ml taurin. Larutan disiapkan setiap hari (baru).
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SNI 01-6684-2002
pertama kemudian kumpulkan 5 – 10 ml saringan berikutnya kedalam botol reaksi g)
Ekstrak ini dapat disimpan ditempat gelap pada suhu 4°C selama 24 jarn sebelum diderivatisasi.
5.2 a)
Derivatisasi Pipet 1,0 ml cairan dari larutan deret standar taurin, ekstrak contoh dan blanko dari (5.1) masukkan ke botol reaksi 5 ml secara terpisah.
b)
Tambahkan 1,0 ml bufer natrium karbonat diikuti dengan 1,0 ml dansil klorida. Sumbat botol reaksi dan aduk isi secara inversi.
c)
Biarkan botol reaksi selama 2 jam ditempat gelap pada suhu 20 ± 3°C, dengan pengadukan tambahan setelah 1 jam. (sampai warna kuning memudar/menjadi pucat sejalan dengan penyerapan pereaksi).
d)
Tambahkan 0,1 ml metilamin hidroklorida untuk mengakhiri reaksi. Campurkan dengan menggunakan vortex mixer dan biarkan ditempat gelap sampai endapan stabil. (Cara lain : saring dengan membran 0,45 µm).
e)
Pindahkan cairan bening secukupnya kedalam botol reaksi. Turunan ini dapat disimpan ditempat gelap pada suhu 4°C sampai selang waktu 48 jam untuk analisis.
A.6 A. 6 a)
Penetap Pene tap an Kondisikan HPLC dengan fasa gerak dengan kecepatan alir 1-2 ml/menit sampai diperoleh garis lurus yang stabil.
b)
Suntikkan 20 µl setiap deret standar taurin .yang telah diderivatisasi pada kondisi isokratik dengan kecepatan alir 1-2 ml/menit, sehingga waktu elusi dansil taurin 10-15 menit.
c)
Biarkan HPLC selama 10 menit untuk fase pembersihan sebelum penyuntikan berikutnya.
d)
Buat kurva kalibra..si minimal terdiri dari 4 titik berdasarkan Iuas atau tinggi puncak (peak). Bila larutan blako standar tidak memberikan titik nol, maka kurva standar dibuat
berdasarkan
perhitungan
regresi
linier
kemiringan kemiringan (slope) dan koefisien koefisien regresi ( r > 0,999).
dengan
menetapkan
besarnya
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SNI 01-6684-2002
dengan pengertian : P Contoh adalah Luas atau tinggi puncak dalam ekstrak contoh ; S
adalah Slope ;
V
adalah Volume contoh ( 100 ml );
W
adalah Bobot contoh ( g ) ;
1000
adalah Faktor konversi dari µg ke mg ;
100
adalah Faktor konversi ke 100 g.
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SNI 01-6684-2002
Lampiran B Kafein B.1 Acuan : AOAC.Offic AOAC. Official ial Method Me thod 962.13 – 1999, 1999 , Cafein in Non Alcoholic Beverages. B.2 Prinsip Kafein
yang
terlarut
dalam
contoh
diekstrak
mengunakan
kloroform,
kemudian
absorbennya diukur dengan spektrofofometer pada panjang gelombang 276 nm. B.3 Pereaksi a.
Larutan pereduksi, larutkan 5 g Na 2SO3 dan 5g KCNS kedalam 100 ml air suling.
b.
Larutan asam fosfat encer : encerkan 15 ml H3PO4 p.a ke dalam 85 ml air suling.
c.
Larutan natrium hidroksida, larutkan 25 g NaOH p.a kedalam 75 ml air suling suling
d.
Larutan standar kafein (1 mg/ml) : larutkan 100 mg kafein murni dalam CHCI 3 dan encerkan sampai 100 ml dengan CHCI 3.
B.4 Peralatan a.
Neraca analitik terkalibrasi.
b.
Spektrofotometer.
c.
Labu kocok/labu pemisah 125 ml,
d.
Corong gelas Ø 7 cm. Pipet gondok 10 ml.
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SNI 01-6684-2002
beberapa menit sampai terlihat jelas batas pisah kedua cairan. c. Alirkan cairan yang berada dibawah, yaitu CHCI 3 melalui corong gelas yang telah diberi kertas saring kedalam labu ukur 100 ml. d.
Ekstraksi diulangi lagi dengan menambahkan 40 mI CHCI 3 dan Ianjutkan seperti di atas (6 c).
e.
Labu kocok dan kertas saring dibilas dengan 3 m; CHCI 3 sebanyak dua kali.
f.
Encerkan cairan ekstrak tadi dengan CHCI 3 sampai batas garis 100 ml.
g.
Ukur absorbansi larutan hasil ekstraksi tadi dengan spektrofotometer spektrofotome ter pada panjang gelombang 276 nrn terhadap CHCI 3.
h.
Tentukan konsentrasi kafein dari kurva standar dengan regresi linier dan hitung kadar kafein dalam contoh (mg/100 ml).
B.7 Perhitungan Kafein (mg/100 mI) =
100 10
xC
dengan pengertian : C adalah konsentrasi kafein dari kurva.
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SNI 01-6684-2002
Lampir an C P em em a n i s b u a t a n C.1 Sakarin C . 1. 1. 1 A c u a n : AO A O A C O f f i c i a l M e t h o d 9 3 4 . 0 4 – 1 9 9 9 , Saccaharin in Nonalcoholic Beverages. C . 1. 1. 2 P r i n s i p Contoh diekstrak dengan eter, direaksikan dengan pereaksi Nessler dan warnanya dibandingkan dengan standar NH 4 CI. C.1.3 Pereaksi a)
Larutan asam kiorida, HCI pa.
b)
Larutan NH 3 – bebas H 2 O .
c)
Eter.
d)
Air suling.
e)
Pereaksi Nessler. HgI 2 dan 70 g KI dengan sedikit air suling. − Larutkan 100 g HgI
− Tambahkan perlahan dengan diaduk larutan dingin 160 g NaOH dalam 500 ml air suling dan encerkan sampai 1 liter.
− Pereaksi stabil selama 1 tahun bila disimpan pada tempat pyrex tanpa kena sinar matahari langsung.
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SNI 01-6684-2002
uapkan larutan sampai menjadi kira-kira 1 ml diatas penangas listrik, aduk dengan konstan. e)
Tambahkan lagi 5 ml dengan NH 3 bebas H 2 0 dan 6 ml HCI dan uapkan menjadi 1 ml.
f)
Encer ncerka kan n sam pai 50 ml den gan NH 3 b e b a s H 2O d a n 2 m l l a r u t a n i n i diencerkan dengan NH 3 bebas H2O menjadi 25 ml.
g)
Tambahkan 1 ml pereaksi Nessler.
h)
B a n d i n g k a n d e n g a n s t a n d a r N H 4CI, seperti biasanya, 0,2921 g NH 4CI = 1 g sa kar in ben tu k tida tidak k . lar laru ut (C 7H 5NO3S) dan 1,317 317 g g aram nat rium (C7H4N NaO3S.2H20).
i)
Seb aik nya bua buat st and ar NH 4CI y a n g s e t a r a d e n g a n 2 0 0 p p m s a k a r i n y a n g tidak larut.
C.1.6 Perhitungan Sakarin (mg/kg) = V x C x A W dengan pengertian : V
adalah volume contoh
C
adalah konsentrasi sakarin dalam contoh
A
adalah faktor fakt or pengencer pen genceran an
W
adalah bobot contoh (g)
C.2 Siklamat
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SNI 01-6684-2002
d)
Kaca arloji.
e)
Cawan Gooch.
f)
Penangas air.
g)
Gelas ukur.
C.2.5 Prosedur a)
Ke dalam 100 ml larutan yang mengandung mengandung 10mg 10mg – 300 mg mg siklamat tambahkan 10 ml lar uta n HCI HCI 10% dan dan lar uta n BaCl BaCl2 1 0 % .
b)
Kocok dan biarkan selama 30 menit, jika timbul endapan saring dan cuci dengan air suling.
c)
Tambah Tambahkan kan 1 0 ml laruta larutan n N a N O 2 10% pada filtrat, kocok dengan pengaduk, dan tutup dengan kaca arloji dan panaskan pada penangas air selama 2 jam atau lebih.
d)
Ad uk en da pa n 3 kali kali deng dengan an sela selang ng wa kt u ½ ja m. An gk at da ri pena penang ngas as d a n biarkan biarkan ditempat ditempat hangat hangat semalam. semalam.
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SNI 01-6684-2002
Detektor : FID (Flame Ionization Detector). Rekorder : 1 mV s t r i p c h a r t . Kolom
: gelas dengan panjang 1,8 m dan diameter 4 mm.
Isi kolom : gas chrom Q ukuran 100 mesh – 200 mesh dengan 10% DC-200. c)
Kondisi operasi. Temperatur kolom
: 200 0C (waktu retensi sortbitol asetat adalah
9-10 menit) Temperatur Injektor
: 230 0C
Temperatur Detektor
: 210 0C
Kecepatan alir g a s pembawa (N 2) : 1 2 0 ml/menit Kecepatan alir udara
: 350 – 400 ml/menit
Kecepatan alir gas hidrogen
: optimal
Sensitivitas Sensitivitas
: 0,4 x 10-9 amp untuk skala defleksi penuh
atau untuk defleksi ½ skala bila turunan asetat setara dengan 2,5 µg sorbitol.
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SNI 01-6684-2002
C.3.7 Penetapan Penetapan a) Pipet 25 ml ekstrak metancl ke dalam labu Erlenmeyer 125 ml. b) Uapkan ekstrak sampai kering pada penangas air di udara terbuka. c) Tambahkan 3 ml piridin dan 10 ml asetat anhidrat d) Hubungkanlabu dengan kondensor udara dan refluks 1 jam pada penangas air. e) Tambahkan 60ml - 80 ml air suling, aduk dan dinginkan. f)
Ekstrak dengan 4 bagian CHCI 3 20 ml dan 1 bagian CHC! 3 15 ml
g) Encerkan sampai batas garis dengan CHCI 3 dalam labu ukur 100 ml. h) Injek kira-kira 5 µI ke kromatografi gas. i)
Hitung % sorbitol sebagai berikut :
C.3.8 C.3.8 Perhitun gan % Sorbitol = (mg dari kurva standar x 0,81)
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