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食品安全国家标准 食品中苯并(a)芘的测定
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GB 5009.27-2016
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标准编号: GB 5009.27-2016 (GB5009.27-2016)
中文名称: 食品安全国家标准 食品中苯并(a)芘的测定
英文名称: Determination of benzo (a) pyrene in foods
行业: 国家标准
中标分类: C53
国际标准分类: 67.040
字数估计: 7,769
发布日期: 2016-12-23
实施日期: 2017-06-23
旧标准 (被替代): GB/T 22509-2008; GB/T 5009.27-2003; NY/T 1666-2008; SC/T 3041-2008
标准依据: National Health and Family Planning Commission Notice No.17 of 2016
发布机构: 中华人民共和国国家卫生和计划生育委员会、国家食品药品监督管理总局
范围: 本标准规定了食品中苯并(a)芘的测定方法。本标准适用于谷物及其制品(稻谷、糙米、大米、小麦、小麦粉、玉米、玉米面、玉米渣、玉米片)、肉及肉制品(熏、烧、烤肉类)、水产动物及其制品(熏、烤水产品)、油脂及其制品中苯并(a)芘的测定。
GB 5009.27-2016: 食品安全国家标准 食品中苯并(a)芘的测定
GB 5009.27-2016 英文名称: Determination of benzo (a) pyrene in foods
中华人民共和国国家标准
1 范围
本标准规定了食品中苯并(a)芘的测定方法。
本标准适用于谷物及其制品(稻谷、糙米、大米、小麦、小麦粉、玉米、玉米面、玉米渣、玉米片)、肉及
肉制品(熏、烧、烤肉类)、水产动物及其制品(熏、烤水产品)、油脂及其制品中苯并(a)芘的测定。
5 分析步骤
5.1 试样制备、提取及净化
5.1.1 谷物及其制品
预处理:去除杂质,磨碎成均匀的样品,储于洁净的样品瓶中,并标明标记,于室温下或按产品包装要求的保存条件保存备用。
提取:称取1g(精确到0.001g)试样,加入5mL正己烷,旋涡混合0.5min,40℃下超声提取
10min,4000r/min离心5min,转移出上清液。再加入5mL正己烷重复提取一次。合并上清液,用
下列2种净化方法之一进行净化。
净化方法1:采用中性氧化铝柱,用30mL正己烷活化柱子,待液面降至柱床时,关闭底部旋塞。将
待净化液转移进柱子,打开旋塞,以1mL/min的速度收集净化液到茄形瓶,再转入50mL正己烷洗
脱,继续收集净化液。将净化液在40℃下旋转蒸至约1mL,转移至色谱仪进样小瓶,在40℃氮气流下
浓缩至近干。用1mL正己烷清洗茄形瓶,将洗涤液再次转移至色谱仪进样小瓶并浓缩至干。准确吸
取1mL乙腈到色谱仪进样小瓶,涡旋复溶0.5min,过微孔滤膜后供液相色谱测定。
净化方法2:采用苯并(a)芘分子印迹柱,依次用5mL二氯甲烷及5mL正己烷活化柱子。将待净
化液转移进柱子,待液面降至柱床时,用6mL正己烷淋洗柱子,弃去流出液。用6mL二氯甲烷洗脱并
收集净化液到试管中。将净化液在40℃下氮气吹干,准确吸取1mL乙腈涡旋复溶0.5min,过微孔滤膜后供液相色谱测定。
5.1.2 熏、烧、烤肉类及熏、烤水产品
预处理:肉去骨、鱼去刺、贝去壳,把可食部分绞碎均匀,储于洁净的样品瓶中,并标明标记,于-16℃~-18℃冰箱中保存备用。
提取:同5.1.1中提取部分。
净化方法1:除了正己烷洗脱液体积为70mL外,其余操作同5.1.1中净化方法1。
净化方法2:操作同5.1.1中净化方法2。
5.1.3 油脂及其制品
提取:称取0.4g(精确到0.001g)试样,加入5mL正己烷,旋涡混合0.5min,待净化。
注:若样品为人造黄油等含水油脂制品,则会出现乳化现象,需要4000r/min离心5min,转移出正己烷层待净化。
净化方法1:除了最后用0.4mL乙腈涡旋复溶试样外,其余操作同5.1.1中的净化方法1。
净化方法2:除了最后用0.4mL乙腈涡旋复溶试样外,其余操作同5.1.1中的净化方法2。
试样制备时,不同试样的前处理需要同时做试样空白试验。
5.2 仪器参考条件
a) 色谱柱:C18,柱长250mm,内径4.6mm,粒径5μm,或性能相当者;
b) 流动相:乙腈+水=88+12;
c) 流速:1.0mL/min;
d) 荧光检测器:激发波长384nm,发射波长406nm;
e) 柱温:35℃;
f) 进样量:20μL。
5.3 标准曲线的制作
将标准系列工作液分别注入液相色谱中,测定相应的色谱峰,以标准系列工作液的浓度为横坐标,
以峰面积为纵坐标,得到标准曲线回归方程。苯并(a)芘标准溶液的液相色谱图见图A.1。
5.4 试样溶液的测定
将待测液进样测定,得到苯并(a)芘色谱峰面积。根据标准曲线回归方程计算试样溶液中苯并(a)芘的浓度。
7 精密度在重复性条件下获得的两次独立测试结果的绝对差值不得超过算术平均值的20%。
8 其他方法检出限为0.2μg/kg,定量限为0.5μg/kg。
附 录 A
苯并(a)芘标准溶液的液相色谱图
苯并(a)芘标准溶液的液相色谱图见图A.1。
GB 5009.27-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard –
Determination of Benzo(a)Pyrene in Foods
ISSUED ON. DECEMBER 23, 2016
IMPLEMENTED ON. JUNE 23, 2017
Issued by. National Health and Family Planning Commission of the
People's Republic of China;
China Food and Drug Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle ... 4
3 Reagents and Materials ... 4
4 Instruments and Apparatus ... 6
5 Analysis Steps ... 6
6 Expression of Analysis Results ... 8
7 Precision ... 9
8 Others ... 9
Appendix A Liquid Chromatogram of Benzo(a)pyrene Standard Solution ... 10
National Food Safety Standard –
Determination of Benzo(a)Pyrene in Foods
1 Scope
This Standard specifies the determination method for the benzo(a)pyrene in foods.
This Standard is applicable to determination of the benzo(a)pyrene of the grains and
their products (rice, brown rice, rice, wheat, wheat flour, corn, cornmeal, corn residues
AND corn flakes), meat and meat products (smoked, roasted and barbecued), aquatic
animals and their products (smoked and boiled aquatic products) AND grease & their
products.
2 Principle
Samples shall be extracted by organic solvents, purified by neutral alumina or
molecularly imprinted cartridges AND concentrated to dryness; use acetonitrile to
dissolve it; it shall be separated by reversed-phase liquid chromatography AND
detected by fluorescence detector. Use the retention time of chromatographic peaks
to determine the quality; use the external standard method to determine the quantity.
3 Reagents and Materials
Unless otherwise stated, the used reagents in this method shall all be analytical purity;
the water shall be the Grade-1 water which is specified in GB/T 6682.
3.1 Reagents
3.1.1 Toluene (C7H8). Chromatographically pure.
3.1.2 Acetonitrile (CH3CN). Chromatographically pure.
3.1.3 n-hexane (C6H14). chromatography.
3.1.4 Dichloromethane (CH2Cl2). Chromatographically pure.
3.2 Standards
Benzo(a)pyrene standard (C20H12, CAS No.. 50-32-8). the purity shall be ≥ 99.0%; or
solution into the chromatograph’s sample vial again; concentrate it until it is near dry.
Accurately pipette 1mL of acetonitrile into the chromatograph’s sample vial, vortex re-
dissolve it for 0.5min; after passing the microporous membrane, it shall be used for
liquid chromatography.
Purification method 2. adopt the benzo(a)pyrene molecular imprinting column; orderly
use 5mL of dichloromethane and 5mL of n-hexane to activate the column. Transfer the
liquid to be purified into the column; when the liquid-level falls to the column bed, use
6mL of n-hexane to rinse the column; discard the effluent. Use 6mL of dichloromethane
to elute and collect the purified solution into the test tube. Under 40°C, use nitrogen to
dry the purification solution; accurately pipette 1mL of acetonitrile; vortex re-dissolve it
for 0.5min; after passing the microporous membrane, it shall be used for liquid
chromatography.
5.1.2 Smoked, roasted & barbecued AND smoked & grilled aquatic products
Pretreatment. remove the bones of the meat; remove the thorns of fish; remove the
shell of shellfish; grind the edible portion evenly; store it in clean sample bottles; mark
it; at -16°C ~ -18°C, stored it in the refrigerator.
Extraction. same as the extraction in 5.1.1.
Purification method 1. Except that the volume of n-hexane’s eluent is 70 mL, the rest
of the operation shall be the same as the purification method 1 in 5.1.1.
Purification method 2. the operation shall be the same as the purification method 2 in
5.1.1.
5.1.3 Grease and its products
Extraction. weigh and take 0.4g (accurate to 0.001g) of sample; add 5mL of n-hexane;
Note. If the samples are the hydrous oil products, such as margarine, etc., emulsification will occur. It
shall perform 4000r/min centrifugalization for 5min; transfer out the n-hexane layer. To be purified.
Purification method 1. Except for using 0.4mL of acetonitrile to vertically re-dissolve
the sample in the last, other operations shall be the same as the purification method 1
in 5.1.1.
Purification method 2. Except for using 0.4mL of acetonitrile to vertically re-dissolve
the sample in the last, other operations shall be the same as the purification method 2
in 5.1.1. When the sample is prepared, pretreatments of different samples need to
have sample’s blank test at the same time.
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