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食品安全国家标准 食品添加剂 山楂核烟熏香味料I号、II号
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GB 1886.127-2016
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标准编号: GB 1886.127-2016 (GB1886.127-2016)
中文名称: 食品安全国家标准 食品添加剂 山楂核烟熏香味料I号、II号
英文名称: National Food Safety Standard -- Food Additives -- Hawthorn nuclear smoked flavouring material I, II
行业: 国家标准
中标分类: X09
字数估计: 12,181
发布日期: 2016-08-31
实施日期: 2017-01-01
标准依据: 国家卫生和计划生育委员会公告2016年第11号
GB 1886.127-2016: 食品安全国家标准 食品添加剂 山楂核烟熏香味料I号、II号
GB 1886.127-2016 英文名称: National Food Safety Standard -- Food Additives -- Hawthorn nuclear smoked flavouring material I, II
1 范围
本标准适用于以山楂核为原料,在800℃以下经干馏(无氧裂解)、冷凝、分离等方法制得的水溶性
食品添加剂山楂核烟熏香味料Ⅰ号、Ⅱ号。
本标准不适用于与水不相溶的油状物及由其制得的产物和由其他材料或其他方法所制得的产物,
如木醋酸等。
2 术语和定义
2.1 山楂核
山楂核经水洗、晒干,具有特有香气和颜色的颗粒状物。不应添加其他木质材料或除去原有香味
成分。
2.2 山楂核烟熏香味料
以山楂核为原料,在800℃以下干馏生成熏烟,将熏烟冷凝,将冷凝物分离精制而成。它是由众多
熏烟成分所组成的复杂混合物。
2.3 山楂核烟熏香味料Ⅰ号
由熏烟冷凝物在常压下蒸馏,收集85℃~110℃、呈淡黄色至橘红色、具有烟熏香味的馏分,称为
山楂核烟熏香味料Ⅰ号。
2.4 山楂核烟熏香味料Ⅱ号
由熏烟冷凝物水相和油相分离后经精制所得的水相部分,可溶于水,呈红棕色至棕褐色,具有烟熏
香味的液体,称为山楂核烟熏香味料Ⅱ号。
3 技术要求
3.1 感官要求
感官要求应符合表1的规定。
表1 感官要求
项 目
要 求
Ⅰ号 Ⅱ号
检验方法
色泽 淡黄色至橘红色 棕红色或棕褐色
状态
易流动液体,存放期间有少量焦油状
物析出
易流动液体
将试样置于一洁净白纸
上,用目测法观察
香气 浓郁天然烟熏香气,兼有鲜咸味感 浓郁天然烟熏香气,烟熏肉样香气 GB/T 14454.2
3.2 理化指标
理化指标应符合表2的规定。
表2 理化指标
项 目
指 标
Ⅰ号 Ⅱ号
检验方法
相对密度(25℃/25℃) 1.010~1.025 1.020~1.060 GB/T 11540
酸含量(以乙酸表示)/% 8.0~14.0 10.0~18.0 GB/T 14455.5
酚含量(以2,6-二甲氧基酚表示)/(mg/mL) 2.5~10.0 6.0~18.0 附录A中A.2
羰基化合物含量(以庚醛表示)/(g/100mL) 3.0~11.0 6.0~17.0 附录A中A.3
重金属(以Pb计)/(mg/kg) ≤ 40 GB 5009.74
总砷(以As计)/(mg/kg) ≤ 3.0 GB 5009.11或GB 5009.76
附 录 A
检 验 方 法
A.1 一般规定
本标准所用试剂和水,在没有注明其他要求时,均指分析纯试剂和GB/T 6682规定的三级水。试
验中所用标准溶液、杂质标准溶液、制剂及制品,在没有注明其他要求时,均按GB/T 601、GB/T 602和
GB/T 603的规定制备。实验中所用溶液在未注明用何种溶剂配制时,均指水溶液。
A.2 酚含量(以2,6-二甲氧基酚表示)的测定---修正吉布斯法
A.2.1 方法提要
烟熏液中的酚类化合物同显色剂2,6-二氢醌氯亚胺(2,6-DcGc)在碱性硼酸-氯化钾缓冲溶液中反
应,形成蓝色靛酚。形成色泽后,在560nm处测定吸光度A,由愈创木酚(或其他已知酚)吸光度标准
曲线定量。本法不能区分各种酚,只能提供以愈创木酚表示的总酚含量。
A.2.2 试剂和材料
A.2.2.1 硼酸-氯化钾缓冲溶液:pH=8.3。0.4mol/L硼酸溶液125mL;0.4mol/L氯化钾溶液
125mL;0.2mol/L氢氧化钠溶液40mL。将上述三种溶液混合,并用水稀释到1000mL。
A.2.2.2 NaOH溶液:6g/L。
A.2.2.3 显色剂溶液:称0.25g的2,6-二氢醌氯亚胺于30mL无水乙醇中,冷却保存。
A.2.2.4 愈创木酚标准溶液:用水制备1μg/mL~20μg/mL标准溶液,用于绘制吸光度A 和愈创木酚
的浓度B(μg/mL)标准曲线。
A.2.2.5 烟熏液样品溶液:取0.5mL山楂核烟熏香味料,用水稀释到1000mL(稀释倍数可视样品浓
度高低而定,以使样品稀释液的吸光度A 在0.2~0.7之间)。
A.2.3 仪器和设备
分光光度计。
A.2.4 分析步骤
A.2.4.1 按指定顺序将下列试剂混合在一起:
a) 硼酸-氯化钾缓冲溶液5mL;
b) 烟熏液样品溶液5mL,或愈创木酚标准溶液5mL,或做空白对照用的水5mL;
c) 用NaOH溶液1mL调节pH到9.8。
A.2.4.2 将1mL显色剂溶液用水稀释到15mL。取1mL稀释液立即加入到混合液中,在室温下使混
合液放置25min后形成色泽,再用1cm比色杯在波长560nm处测定吸光度A。
A.2.4.3 绘制吸光度A 对于愈创木酚浓度B(μg/mL)的标准曲线(直线)。
A.2.5 结果计算
ρ1=
B1×D×Mr1
1000×Mr2
(A.1)
式中:
B1 ---从标准曲线上读得的吸光度A 的对应值(以愈创木酚表示),单位为毫克每毫升(mg/mL);
D ---样品的稀释倍数;
Mr1 ---2,6-二甲氧基酚的相对分子质量;
1000---换算系数;
A.3 羰基化合物含量(以庚醛表示)的测定
A.3.1 第一法:盐酸羟胺法
A.3.1.1 试剂和材料
A.3.1.1.1 氢氧化钾溶液:0.1mol/L。
A.3.1.1.2 盐酸羟胺溶液:0.5mol/L溶液(存放期不超过二周)。称40g盐酸羟胺,加水200mL溶解
后再稀释到1000mL,用盐酸或氢氧化钾溶液调节pH到3(与样品的pH相接近,用pH计检测)。
A.3.1.2 仪器和设备
A.3.1.2.1 酸度计。
A.3.1.2.2 磁力搅拌器。
A.3.1.3.1 空白试验:用移液管吸取25mL盐酸羟胺溶液于磨口锥瓶中,盖上瓶塞,静置2h。用100mL
蒸馏水稀释后,用0.1mol/L氢氧化钾溶液滴定到终点,pH=4.0。
A.3.1.3.2 样品滴定:精确吸取2mL样品于磨口锥形瓶中,重复A.3.1.3.1操作。
A.3.1.4 结果计算
羰基化合物含量ρ2(以庚醛表示),以克每百毫升(g/100mL)计,按式(A.2)计算:
ρ2=
M ×c×(V-V0)
(A.2)
式中:
c ---氢氧化钾溶液浓度,单位为摩尔每升(mol/L);
V ---滴定样品消耗的氢氧化钾溶液体积,单位为毫升(mL);
V0---空白滴定消耗的氢氧化钾溶液体积,单位为毫升(mL);
20---换算系数。
平行试验结果的相对误差不大于1%。
A.3.2 第二法:修正的兰谱-克拉克法(Modifiedlappan-ClarkMethod)(仲裁法)
A.3.2.1 方法提要
在酸性介质于60℃转化成红色的腙的衍生物,在430nm测定吸光度A,从而计算羰基化合物的含量
(以庚醛或其他已知醛表示)。
A.3.2.2.1 不含羰基化合物的甲醇:在甲醇中加入1%的2,4-DNPH,滴加几滴盐酸,回流3h后蒸馏。
A.3.2.2.2 2,4-DNPH饱和溶液:2,4-DNPH用不含羰基化合物的甲醇溶解,并稀释,使含量达0.05%,
摇动1h或预先24h制备。应有不溶解的2,4-DNPH析出,过滤后使用,保存期为一周。
A.3.2.2.3 氢氧化钾溶液:20mL水中加入10g氢氧化钾,再用不含羰基化合物的甲醇稀释到
100mL。
A.3.2.2.4 2-丁酮标准溶液:用不含羰基化合物的甲醇制备10mg/100mL2-丁酮标准溶液,供绘制吸
光度A-2-丁酮浓度(mg/100mL)标准曲线用。
A.3.2.2.5 0.05%试样溶液:取1mL试样溶液,用水稀释到200mL。取1mL稀释液,再用不含羰基
化合物的甲醇稀释到10mL(总稀释比为1∶2000)。
分光光度计。
A.3.2.4 分析步骤
A.3.2.4.1 向三个量筒中各加入1mL2,4-DNPH,然后第一个量筒中加入1mL样品溶液,第二个量
筒中加入1mL2-丁酮标准溶液,第三个量筒中加入1mL不含羰基化合物的甲醇作空白对照用。
A.3.2.4.2 向所有量筒中准确加入0.05mL盐酸,充分混合,放在50℃的水浴中加热30min。
A.3.2.4.3 迅速冷却后,向各量筒加入5mL氢氧化钾溶液。
A.3.2.4.4 用不含羰基化合物的甲醇稀释每个量筒内的液体混合物到25mL。
A.3.2.4.5 15min后,在480nm下空白对照组甲醇的吸光度A 应为“0”,测定样品或2-丁酮标准液的
吸光度A。
GB 1886.127-2016
GB
NATIONAL STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
National food safety standard – Food additives –
Hawthorn nuclear smoked flavoring material I, II
ISSUED ON. AUGUST 31, 2016
IMPLEMENTED ON. JANUARY 01, 2017
Issued by. National Health and Family Planning Commission of the PRC
3. No action is required - Full-copy of this standard will be automatically &
immediately delivered to your EMAIL address in 0~60 minutes.
Table of contents
1 Scope ... 3
2 Terms and definitions ... 3
3 Technical requirements ... 3
Appendix A Testing method ... 5
National food safety standard – Food additives –
Hawthorn nuclear smoked flavoring material I, II
1 Scope
This standard applies to the water-soluble hawthorn nuclear smoked flavoring
material I and II which uses the hawthorn nuclear as the raw material AND is
produced by such methods as dry distillation (anaerobic cracking),
condensation, separation and other methods at the temperature of not more
than 800 °C.
This standard does not apply to the products manufactured by the
water-insoluble oily substances and their products and other materials or by
other methods, such as wood acid and the like.
2 Terms and definitions
2.1 Hawthorn nucleus
It refers to the particles produced by water washing and natural drying of the
hawthorn nucleus which has a unique aroma and color. It shall not add other
wood material or ingredients which may remove the original flavor.
2.2 Hawthorn nucleus smoked flavoring material
It refers to the product using the hawthorn nuclear as raw material which is
subjected to dry distillation at 800 °C to produce fumigation, that is further
condensed, separated, and refined. It is a complex compound which is
composed of multiple smoked ingredients.
2.3 Hawthorn nucleus smoked flavoring material I
It refers to the fraction which is collected at 85 °C ~ 110 °C from the distillation
of smoked condensate at normal pressure, is in light yellow to orange, AND
has the smoked flavor.
2.4 Hawthorn nucleus smoked flavoring material II
It refers to the aqueous phase portion as refined from the smoked condensate
after separation between water phase and oil phase. It is soluble in water, has
the reddish brown to tan color, and has the smoked flavor.
3 Technical requirements
3.1 Sensory requirements
Sensory requirements shall comply with the requirements of Table 1.
Appendix A
Testing method
A.1 General provisions
The reagents and water used in this standard, unless otherwise specified,
refers to the analytical pure reagents and the level III water as specified in
GB/T 6682. The standard solutions, impurity standard solutions, preparations
and products used in the tests shall be prepared in accordance with the
provisions of GB/T 601, GB/T 602 and GB/T 603, unless otherwise specified.
The solution used in the test, unless otherwise specified of the solvent, refers
to the aqueous solution.
A.2 Determination of phenol content (expressed as 2,6-dimethoxyphenol)
- modified Gibbs method
A.2.1 Method summary
The phenolic compounds in the smoked solution react with the colorant
2,6-dihydroquinone chloroimine (2,6-DcGc) in alkaline boric acid-potassium
chloride buffer to form blue indophenol. After forming the color, the absorbance
A is measured at 560 nm AND it is quantified by the absorbance standard
curve of guaiacol (or other known phenol). This method cannot distinguish
between the various phenols, BUT can only provide the total phenol content of
guaiacol.
A.2.2 Reagents and materials
A.2.2.1 Boric acid-potassium chloride buffer solution. pH = 8.3. 125 mL of 0.4
mL of 0.2 mol/L sodium hydroxide solution. MIX these three solutions; USE
water to dilute it to 1000 mL.
A.2.2.2 NaOH solution. 6 g/L.
A.2.2.3 Developer solution. WEIGH 0.25 g of 2,6-dihydroquinone chloride
imine in 30 mL of absolute ethanol; COOL it before storage.
A.2.2.4 Guaiacol standard solution. USE water to prepare 1 μg/mL ~ 20 μg/mL
standard solution, to draw the standard curve of absorbance A and the
guaiacol concentration B (μg/mL).
A.2.2.5 Smoked sample solution. TAKE 0.5 mL of hawthorn nuclear smoked
concentration of sample, so that the absorbance A of the sample dilution is
between 0.2 ~ 0.7).
The total carbonyl compound in the smoked flavor material and the
2,4-dinitrophenyl hydrazine (abbreviated as 2,4-DNPH) are converted to a red
hydrazone derivative at 60 °C in an acidic medium, AND the absorbance A is
measured at 430 nm, so as to calculate the content of the carbonyl compound
(expressed as heptanal or other known aldehydes).
A.3.2.2 Reagents and materials
A.3.2.2.1 Methanol free of carbonyl compounds. ADD 1% 2,4-DNPH into
DISTILL it.
A.3.2.2.2 2,4-DNPH saturated solution. USE the methanol free of carbonyl
compounds to dissolve 2,4-DNPH; DILUTE it to make its content reach to
0.05%; SHAKE it for 1 h or PREPARE it 24 h in advance. It shall have the
precipitation of insoluble 2,4-DNPH; FILTER and PRESERVE it, AND the shelf
life is one week.
A.3.2.2.3 Potassium hydroxide solution. ADD 10 g of potassium hydroxide into
20 mL of water; USE the methanol free of carbonyl compounds to dilute it to
100 mL.
compounds to prepare 10 mg/100 mL of 2-butanone standard solution, which
is used to draw the standard curve of absorbance A-2-butanone concentration
(mg/100 mL).
A.3.2.2.5 0.05% sample solution. TAKE 1 mL of sample solution; USE water to
dilute it to 200 mL. TAKE 1 mL of dilution; USE the methanol free of carbonyl
compounds to dilute it to 10 mL (total dilution ratio 1.2000).
A.3.2.3 Instruments and equipment
Spectrophotometer.
A.3.2.4 Analytical procedures
Then ADD 1 mL of sample solution into the first measuring cylinder. ADD 1 mL
of 2-butanone standard solution into the second measuring cylinder. ADD 1 mL
of methanol free of carbonyl compound into the third measuring cylinder as the
blank control.
A.3.2.4.2 Accurately ADD 0.05 mL of hydrochloric acid to all measuring
cylinders; MIX it thoroughly; PLACE it in a 50 °C water bath to heat it for 30
min.
A.3.2.4.3 After rapid cooling, ADD 5 mL of potassium hydroxide solution into
each measuring cylinder.
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