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食品安全国家标准 食品中铝的测定
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GB 5009.182-2017
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标准编号: GB 5009.182-2017 (GB5009.182-2017)
中文名称: 食品安全国家标准 食品中铝的测定
英文名称: Food safety national standard -- Determination of aluminum in food
行业: 国家标准
中标分类: X09
字数估计: 11,186
发布日期: 2017-04-06
实施日期: 2017-10-06
旧标准 (被替代): GB/T 5009.182-2003; GB/T 23374-2009; GB/T 18932.11-2002部分; SN/T 2208-2008部分
标准依据: State Health and Family Planning Commission Notice No. 5 of 2017
GB 5009.182-2017: 食品安全国家标准 食品中铝的测定
GB 5009.182-2017 英文名称: Food safety national standard -- Determination of aluminum in food
中华人民共和国国家标准
1 范围
本标准规定了食品中铝含量测定的分光光度法、电感耦合等离子体质谱法、电感耦合等离子体发射
光谱法和石墨炉原子吸收光谱法。
本标准第一法适用于检测使用含铝食品添加剂的食品中的铝,第二法、第三法和第四法适用于检测食品中的铝。
第一法 分光光度法
4 仪器和设备注:所有玻璃仪器均需以硝酸(1+5)浸泡24h以上,用自来水反复冲洗,最后用水冲洗晾干后方可使用。
4.1 分光光度计。
4.2 天平:感量1mg。
4.3 可调式控温电热炉或电热板。
4.4 酸度计(±0.1pH)。
4.5 恒温干燥箱。
5 分析步骤
5.1 试样制备
在采样和试样制备过程中,应注意不使试样污染,应避免使用含铝器具。
面制品、豆制品、虾味片、烘焙食品等样品粉碎均匀后,取约30g置85℃恒温干燥箱中干燥4h。
5.2 试样消解
称取试样0.2g~3g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于硬质玻璃消
化管或锥形瓶中,加入10mL硝酸,0.5mL硫酸,在可调式控温电热炉或电热板上加热,推荐条件:100℃
加热1h,升至150℃加热1h,再升至180℃加热2h,然后升至200℃,若变棕黑色,再补加硝酸消化,
直至管口冒白烟,消化液呈无色透明或略带黄色。取出冷却,用水转移定容至50mL(V1)容量瓶中,混
匀备用。同时做试剂空白试验。
5.3 显色反应及比色测定
分别吸取1.00mL(V2)试样消化液、空白溶液分别置于25mL具塞比色管中,加水至10mL刻度。
另取25mL具塞比色管7支,分别加入铝标准使用溶液0mL、0.500mL、1.00mL、2.00mL、3.00mL、
4.00mL和5.00mL(该系列标准溶液中铝的质量分别为0μg、0.500μg、1.00μg、2.00μg、3.00μg、
4.00μg、5.00μg),并依次向各管中加入硫酸溶液(1%)1mL,加水至10mL刻度。
向标准管、试样管、试剂空白管中滴加1滴对硝基苯酚乙醇溶液(1g/L),混匀,滴加氨水溶液(1+1)
至浅黄色,滴加硝酸溶液(2.5%)至黄色刚刚消失,再多加1mL,加入1mL抗坏血酸溶液(10g/L),混
匀后加3mL铬天青S溶液(1g/L),混匀后加1mLTritonX-100溶液(3%),3mLCPB溶液(3g/L),
3mL乙二胺-盐酸缓冲溶液,加水定容至25.0mL,混匀,放置40min。
于620nm波长处,用1cm比色皿以空白溶液为参比测定吸光度值。以标准系列溶液中铝的质量
为横坐标,以相应的吸光度值为纵坐标,并绘制标准曲线。根据试样消化液的吸光度值与标准曲线比较定量。
7 精密度在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的10%。
8 其他当称样量为1g(或1mL),定容体积为50mL时,方法的检出限为8mg/kg(或8mg/L),定量限为25mg/kg(或25mg/L)。
第二法 电感耦合等离子体质谱法见GB 5009.268。
第三法 电感耦合等离子体发射光谱法见GB 5009.268。
第四法 石墨炉原子吸收光谱法
9 原理
试样消解处理后,经石墨炉原子化,在257.4nm处测定吸光度。在一定浓度范围内铝含量与吸光
度值成正比,与标准系列比较定量。
10 试剂和材料
除非另有说明,所用试剂为优级纯,试验用水为GB/T 6682规定的二级水。
10.1 试剂
10.1.1 硝酸(HNO3)。
10.1.2 硫酸(H2SO4)。
10.2 试剂配制
10.2.1 硝酸溶液(1+99):吸取1mL硝酸加入99mL水中,混匀。
10.2.2 硝酸溶液(5+95):量取5mL硝酸加入95mL水中,混匀。
10.3 标准品铝标准溶液:1000mg/L。或经国家认证并授予标准物质证书的一定浓度的铝标准溶液。
10.4 标准溶液配制
10.4.1 铝标准中间液(100mg/L):准确吸取1.00mL铝标准溶液(1000mg/L)于10mL容量瓶中,
加硝酸溶液(5+95)定容至刻度,混匀。
10.4.2 铝标准使用液(1.00mg/L):准确吸取1.00mL铝标准中间液(100mg/L),置于100mL容量
瓶中,用硝酸溶液(5+95)稀释至刻度,混匀后再从中准确吸取1.00mL于100mL容量瓶中,用水稀释至刻度,混匀。
10.4.3 铝标准系列溶液:分别吸取铝标准使用液(1.00mg/L)0mL、2.50mL、5.00mL、10.0mL、
15.0mL和20.0mL于100mL容量瓶中,加硝酸溶液(1+99)至刻度,混匀。此铝标准系列溶液的质
量浓度分别为0μg/L、25.0μg/L、50.0μg/L、100μg/L、150μg/L和200μg/L。
11 仪器和设备
注:所有玻璃仪器、消解罐均需以硝酸(1+5)浸泡24h以上,用自来水反复冲洗,最后用水冲洗晾干后方可使用。
11.1 石墨炉原子吸收光谱仪:附铝空心阴极灯。
11.2 天平:感量1mg。
11.3 可调式控温电热炉。
11.4 可调式电热板。
11.5 微波消解仪:配聚四氟乙烯消解内罐。
11.6 压力消解罐:配聚四氟乙烯消解内罐。
11.7 恒温干燥箱。
12 分析步骤
12.1 试样制备
注:在采样和试样制备过程中,应避免污染,应避免使用含铝器具。
12.1.1 粮食、豆类样品
样品去除杂物后,粉碎,储于塑料瓶中。
12.1.2 蔬菜、水果、鱼类、肉类等水分含量高的样品
样品用水洗净,晾干,取可食部分,制成匀浆,储于塑料瓶中。
12.1.3 饮料、酒、醋、酱油等液体样品将样品摇匀。
12.1.4 面制品、豆制品、虾味片、烘焙食品等样品
样品粉碎均匀后,取约30g置85℃恒温干燥箱中干燥4h。
12.2 试样消解
称取固体试样0.2g~3g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于硬质玻
璃消化管中,加入10mL硝酸,0.5mL硫酸,在可调式控温电热炉上加热,推荐条件:100℃加热1h,升
至150℃加热1h,再升至180℃加热2h,然后升至200℃,若变棕黑色,再补加硝酸消化。直至管口冒
白烟,消化液呈无色透明或略带黄色。取出冷却,用水转移定容至25mL容量瓶,混匀备用,同时做试
剂空白试验。亦可采用锥形瓶,于可调式电热板上,按上述操作方法进行湿式消解。
12.2.2 微波消解
称取固体试样0.2g~0.8g(精确至0.001g)或准确移取液体试样0.500mL~3.00mL,置于微波
消解内罐中,加入硝酸5mL~8mL,盖上内罐盖,然后旋紧外盖置于微波消解仪中,根据不同种类的试
样设置微波炉消解系统的消解条件(具体消解条件参考附录A),消解完毕待消解罐冷却至室温后,打开
量瓶中,用水定容至刻度,混匀备用,同时做试剂空白试验。
12.2.3 压力罐消解
称取固体试样0.2g~1g(精确至0.001g)或准确移取液体试样0.500mL~5.00mL,置于压力消
解内罐中,加入硝酸5mL~8mL,盖上内盖,旋紧外套,置于恒温干燥箱中,消解完毕待消解罐冷却至室温
后,打开压力消解罐,取出内罐,在电热板上赶酸至近干,待降至室温后用少许水洗涤消化罐3次~4次,
洗液合并于25mL容量瓶中,用水定容至刻度,混匀备用,同时做试剂空白试验(具体消解条件参考附录B)。
12.3 测定
12.3.1 仪器参考条件
根据各自仪器性能调至最佳状态。参考条件为波长257.4nm,狭缝0.5nm,灯电流10mA~
2750℃,持续4s~5s;内气流量0.3L/min,进样量10μL,原子化时停气。
12.3.2 标准曲线制作
按质量浓度由低到高的顺序将10μL标准系列溶液(可根据使用仪器选择最佳进样量)注入石墨
管,原子化后测其吸光度值。以质量浓度为横坐标,吸光度值为纵坐标,制作标准曲线。
12.3.3 试样溶液的测定
按仪器最佳进样量将适当体积的试样消化液、空白溶液分别注入石墨炉中,测定其吸光度值,由标
准曲线得到试样消化液中中铝的质量浓度。
14 精密度在重复性条件下获得的两次独立测定结果的绝对差值不得超过算术平均值的20%。
15 其他
定量限为0.8mg/kg(或0.8mg/L)。
附 录 A
微波消解升温程序
微波消解升温程序见表A.1。
GB 5009.182-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard -
Determination of aluminum in foods
ISSUED ON. APRIL 6, 2017
IMPLEMENTED ON. OCTOBER 6, 2017
Issued by. National Health and Family Planning Commission of the PRC;
China Food and Drug Administration.
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
Foreword ... 3
1 Scope .. 4
2 Principles ... 4
3 Reagents and materials .. 4
4 Instrument and equipment .. 6
5 Analytical procedures ... 7
6 Analysis results expression ... 8
7 Precision... 8
8 Others ... 8
9 Principles ... 9
10 Reagents and materials... 9
11 Instrument and equipment ... 10
12 Analytical procedures .. 10
13 Analysis results expression .. 13
14 Precision .. 13
15 Others ... 13
Appendix A Microwave digestion temperature-rise program ... 14
Appendix B Pressure-tank digestion reference heating conditions .. 15
Foreword
For the determination method of aluminum, this standard replaces GB/T
5009.182-2003 “Determination of aluminum in flour products”, GB/T 23374-
2009 “Determination of aluminium in foods - Inductively coupled plasma mass
spectrometry”, GB/T 18932.11-2002 “Method for the determination of
potassium, phosphorus, iron, calcium, zinc, aluminium, sodium, magnesium,
boron, manganese, copper, barium, titanium, vanadium, nickel, cobalt,
chromium contents in honey. Inductively coupled plasma atomic emission
spectrometric method (ICP-AES)”, SN/T 2208-2008 “Determination of sodium,
magnesium, aluminium, calcium, chromium, iron, nickel, copper, zinc, arsenic,
strontium, molybdenum, cadmium, lead, mercury, selenium, in aquatic products
- Microwave digestion - ICP/MS method ".
As compared with GB/T 5009.182-2003, the main changes of this standard are
as follows.
---The standard name is changed to “National food safety standard -
Determination of aluminium in foods";
---Improve method I spectrophotometry;
---Add inductively coupled plasma mass spectrometry as method II;
---Add inductively coupled plasma emission spectrometry as method III;
---Add graphite furnace atomic absorption spectrometry as method IV.
National food safety standard -
Determination of aluminum in foods
1 Scope
This standard specifies some methods for determination of aluminum content
in foods, such as spectrophotometry, inductively coupled plasma mass
spectrometry, inductively coupled plasma emission spectrometry and graphite
furnace atomic absorption spectrometry.
Method I in this standard applies to the detection of aluminum in foods
containing aluminum-based food additives. Method II, method III and method
IV are applicable to the detection of aluminum in foods.
Method I. Spectrophotometry
2 Principles
After the sample is treated, it is in ethylenediamine-HCl buffer solution (pH 6.7-
7.0), with the existence of Triton X-100 and cetylpyridinium bromide (CPB),
trivalence aluminum ion reacts with chrome azurol S to generate blue-green
quaternary micelle. The absorbance value is measured at a wavelength of 620
nm and compared with the standard series for quantitation.
3 Reagents and materials
Unless otherwise indicated, the reagents used in this method are analytical
3.1 Reagents
3.1.1 Nitric acid (HNO3). guaranteed reagent.
3.1.2 Sulfuric acid (H2SO4). guaranteed reagent.
3.1.3 Hydrochloric acid (HCl). guaranteed reagent.
3.1.4 Ammonium hydroxide (NH3 • H2O). guaranteed reagent.
3.1.5 Anhydrous ethanol (C2H6O). guaranteed reagent.
3.1.6 P-nitrophenol (C6H5NO3).
3.1.7 Chrome azurol S (C23H13O9SCl2Na3).
3.1.8 Ethylenediamine (C2H8N2).
3.1.10 Cetylpyridinium bromide (CPB, C21H38BrN).
3.1.11 Ascorbic acid (C6H8O6).
3.2 Reagent preparation
3.2.1 Hydrochloric acid solution (1+1). MEASURE 50 mL of hydrochloric acid;
MIX it uniformly with 50 mL of water.
3.2.2 Sulfuric acid solution (1%). PIPETTE 1 mL of sulfuric acid; POUR slowly
into 80 mL of water; USE water to dilute it to 100 ml after cooling; MIX it
uniformly.
3.2.3 P-nitrophenol ethanol solution (1 g/L). WEIGH 0.1 g of p-nitrophenol;
3.2.4 Nitric acid solution (5%). MEASURE 5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.5 Nitric acid solution (2.5%). MEASURE 2.5 mL of nitric acid; ADD water to
dilute it to 100 mL; MIX it uniformly.
3.2.6 Ammonium hydroxide solution (1+1). MEASURE 10 mL of ammonium
hydroxide; POUR into 10 mL of water; MIX it uniformly.
3.2.7 Nitric acid solution (2+98). MEASURE 2 mL of nitric acid; MIX it uniformly
with 98 mL of water.
3.2.8 Ethanol solution (1+1). MEASURE 50 mL of anhydrous ethanol;
3.2.9 Chrome azurol S solution (1 g/L). WEIGH 0.1 g of chrome azurol S;
DISSOLVE it in 100 mL of ethanol solution (1+1); MIX it uniformly.
3.2.10 TritonX-100 solution (3%). PIPETTE 3 mL of TritonX-100; PLACE it into
100 mL volumetric flask; ADD water to dilute it to the mark; MIX it uniformly.
3.2.11 CPB solution (3 g/L). WEIGH 0.3 g of CPB; DISSOLVE it in 15 mL of
anhydrous ethanol; ADD water to dilute it to 100 mL; MIX it uniformly.
5 Analytical procedures
5.1 Sample Preparation
In the process of sampling and sample preparation, pay attention not to
After crushing the samples of flour products, bean products, shrimp flavorings
and bakery products uniformly, TAKE out 30 g of sample; PLACE it into
constant-temperature oven at 85°C for 4h.
5.2 Sample digestion
WEIGH 0.2 g ~ 3 g of sample (accurate to 0.001g) or accurately MOVE 0.500
mL ~ 5.00 mL of liquid sample into hard glass digestion tube or conical flask;
ADD 10 mL of nitric acid and 0.5 mL of sulfuric acid; HEAT it on adjustable
temperature-control electric furnace or hot plate, reference conditions. heat it at
100°C for 1h; rise to 150°C and heat it for 1h; rise to 180°C and heat it for 2h;
until the tube mouth emits white smoke, digestive juice is colorless and
transparent or slightly yellow. TAKE it out; after cooling, USE water to transfer
and dilute it to 50 mL (V1) volumetric flask; MIX it uniformly for spare-use.
Meanwhile, DO a reagent blank test.
5.3 Color reaction and colorimetric determination
Respectively PIPETTE 1.00 mL (V2) of sample digestive juice and blank
solution; PLACE them into 25 mL plugged colorimetric tube; ADD water to 10
mL. In addition, TAKE seven 25 mL plugged colorimetric tubes; ADD
respectively aluminum standard working solution 0 mL, 0.500 mL, 1.00 mL,
mass of aluminum is 0 μg, 0.500 μg, 1.00 μg, 2.00 μg, 3.00 μg, 4.00 μg, 5.00
μg respectively); ADD 1 mL of sulfuric acid solution (1%) in each tube
successively; ADD water to 10 mL.
ADD dropwise 1 drop of p-nitrophenol ethanol solution (1 g/L) into standard
tube, sample tube and reagent blank tube; MIX it uniformly; ADD dropwise
ammonium hydroxide solution (1+1) until the solution is light yellow; ADD
dropwise nitric acid solution (2.5%) until the yellow just disappears; ADD again
1 mL of nitric acid solution; ADD 1 mL of ascorbic acid solution (10 g/L); after
mixing it uniformly, ADD 3 mL of chrome azurol S solution (1 g/L); after mixing
g/L), 3 mL of ethylenediamine - hydrochloric acid buffer solution; ADD water to
dilute it to 25.0 mL; MIX it uniformly; PLACE it for 40min.
10.4 Standard solution preparation
10.4.1 Aluminum standard intermediate solution (100 mg/L). Accurately
PIPETTE 1.00 mL of aluminum standard solution (1000 mg/L) into 10 mL
volumetric flask; ADD nitric acid solution (5+95) to dilute it to the mark; MIX it
uniformly.
10.4.2 Aluminum standard working solution (1.00 mg/L). Accurately PIPETTE
1.00 mL of aluminum standard intermediate solution (100 mg/L) into 100 mL
mixing it uniformly, PIPETTE accurately 1.00 mL from the solution; PLACE it
into 100 mL volumetric flask; USE water to dilute it to the mark; MIX it uniformly.
10.4.3 Aluminum standard series solution. PIPETTE respectively aluminum
standard solution (1.00 mg / L) 0 mL, 2.50 mL, 5.00 mL, 10.0 mL, 15.0 mL and
20.0 mL into 100 mL volumetric flask; ADD nitric acid solution (1+99) to the
mark; MIX it uniformly. The mass concentration of the aluminum standard
solution is 0 μg/L, 25.0 μg/L, 50.0 μg/L, 100 μg/L, 150 μg/L and 200 μg/L
respectively.
11 Instrument and equipment
(1+5) for more than 24h, washed repeatedly with tap water, finally rinsed with
water. Dry it by airing before use.
11.1 Graphite Furnace Atomic Absorption Spectrometer. Attached aluminum
hollow cathode lamp.
11.2 Balance. sensitivity is 1 mg.
11.3 Adjustable temperature-control electric furnace.
11.4 Adjustable hot plate.
11.5 Microwave digestion instrument. equipped with Teflon digestion inner-tank.
11.6 Pressure digestion pot. equipped with Teflon digestion inner-tank.
12 Analytical procedures
12.1 Sample preparation
temperature, OPEN the digestion tank; CATCH-acid to dry on electric hot plate;
when it is reduced to room temperature, USE a small amount of water to wash
the digestion tank for 3~4 times; COMBINE washing liquid in 25 mL volumetric
flask; Use water to dilute it to the mark; MIX it uniformly for spare-use.
Meanwhile, DO a sample blank test.
12.2.3 Pressure-tank digestion
WEIGH 0.2 g ~ 1 g of solid sample (accurate to 0.001 g) or accurately MOVE
mL~ 8mL of nitric acid; COVER inner-cap; TIGHTEN outer-sheath; PLACE it
into constant-temperature oven; after digestion tank is cooled to room
temperature, OPEN the pressure digestion tank; TAKE out inner-tank; CATCH-
acid to dry on electric hot plate; when it is reduced to room temperature, USE
a small amount of water to wash the digestion tank for 3~4 times; COMBINE
washing liquid in 25 mL volumetric flask; Use water to dilute it to the mark; MIX
it uniformly for spare-use. Meanwhile, DO a sample blank test. (specific
digestion conditions refer to Appendix B).
12.3 Determination
Adjust to optimum state according to performance of each instrument. The
reference conditions are a wavelength of 257.4 nm, a slit of 0.5 nm, a lamp
current of 10 mA ~ 15 mA, a drying temperature of 85° C. ~ 120° C. for 30 s; an
ashing temperature of 1000° C. ~ 1200° C. for 15 s to 20 s; an atomization
temperature of 2750° C. for 4s ~ 5s; internal gas flow 0.3 L/min, the injection
volume 10 μL, stop gasification during atomization.
12.3.2 Drawing of standard curve
LEAD 10 μL of standard series solution (select the best injection volume
according to instrumentation) into graphite tube from low to high according to
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