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食品安全国家标准 食品接触材料及制品 食品接触用纸中多氯联苯的测定
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GB 31604.39-2016
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标准编号: GB 31604.39-2016 (GB31604.39-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 食品接触用纸中多氯联苯的测定
英文名称: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of Polychlorobiphenyls (PCBs) in Food Contact Paper
行业: 国家标准
中标分类: X09
字数估计: 12,169
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2200-2008
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.39-2016: 食品安全国家标准 食品接触材料及制品 食品接触用纸中多氯联苯的测定
GB 31604.39-2016 英文名称: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of Polychlorobiphenyls (PCBs) in Food Contact Paper
1 范围
本标准规定了食品接触用纸中多氯联苯的气相色谱测定方法及气相色谱-质谱测定方法。
本标准第一法为气相色谱法,第二法为气相色谱-质谱法,均适用于各类食品接触用纸中8种多氯
联苯的测定。
第一法 气相色谱法
2 原理
单层食品接触用纸中的多氯联苯采用正己烷-二氯甲烷混合溶液水浴振荡提取或快速溶剂萃取仪
提取;复合食品接触用纸中的多氯联苯采用快速溶剂萃取仪提取。提取液经浓缩,浓硫酸磺化处理后,
用配有电子捕获检测器的气相色谱仪进行检测,内标法定量。
3 试剂和材料
除非另有说明,本方法所用试剂均为分析纯,水为GB/T 6682规定的一级水。
3.1 试剂
3.1.1 正己烷(C6H14):色谱纯。
3.1.2 二氯甲烷(CH2Cl2)。
3.1.3 乙腈(CH3CN):色谱纯。
3.1.4 浓硫酸(H2SO4):优级纯。
3.2 试剂配制
3.2.1 正己烷-二氯甲烷混合液(1+1):量取100mL正己烷和100mL二氯甲烷,混匀。
3.3 标准品
2,2',5-三氯联苯(PCB18)、2,4,4'-三氯联苯(PCB28)、2,2',5,5'-四氯联苯(PCB52)、2,2',4,5,
5'-五氯联苯(PCB101)、2,3',4,4',5-五氯联苯(PCB118)、2,2',3,4,4',5'-六氯联苯(PCB138)、2,2',
4,4',5,5'-六氯联苯(PCB153)、2,2',3,4,4',5,5'-七氯联苯(PCB180)、内标物2,2',3,3',4,4',5,5',
6,6'-十氯联苯(PCB209):标准品的纯度均≥98%或经国家认证并授予标准物质证书的标准物质。
8种多氯联苯及内标物的相关信息见表A.1。
3.4 标准溶液配制
3.4.1 多氯联苯及内标物标准储备溶液:准确称取适量的多氯联苯标准品,分别用正己烷配制成浓度
为200mg/L的溶液;-18℃密封保存,保存期12个月。
3.4.2 混合标准工作溶液:分别准确吸取适量8种多氯联苯标准储备溶液,用正己烷逐级稀释成
1.00mg/L的混合标准工作溶液;-18℃密封保存,保存期3个月。
3.4.3 内标物工作液:准确吸取适量的内标物(PCB209)标准储备溶液,用正己烷配制成浓度为
1.00mg/L的溶液;-18℃密封保存,保存期3个月。
3.4.4 混合标准系列溶液:吸取适量的混合标准工作溶液和内标物工作液,用正己烷配成浓度为
0.0050mg/L、0.010mg/L、0.025mg/L、0.050mg/L、0.100mg/L和0.200mg/L的混合标准系列溶
液(内标物浓度均为0.050mg/L)。现配现用。
3.5 材料
3.5.1 尼龙滤膜:0.22μm。
3.5.2 硅藻土担体G:优级,CAS号68855-54-9,使用前在400℃马弗炉中加热4h,备用。
4 仪器和设备
4.1 气相色谱仪(GC):配有电子捕获检测器。
4.2 水浴振荡器。
4.3 快速溶剂萃取仪(ASE)。
4.4 天平:感量0.01g和0.00001g。
4.5 离心机:转速≥5000r/min。
4.6 旋转蒸发仪。
4.7 氮吹浓缩仪。
4.8 涡旋振荡器。
5 分析步骤
5.1 取样
按照GB/T 450或GB/T 740取样。取样后应用铝箔包裹样品,以防止样品在测试前发生任何
改变。
5.2 试样的制备
取一份代表性样品(约100g),剪成5mm×5mm以下的碎片,混合均匀。取样后用铝箔包裹,确
保试样不受污染。
5.3 试样的提取
5.3.1 水浴振荡提取(适用于单层食品接触用纸)
称取约2g(精确至0.01g)样品于50mL具塞玻璃离心管中,加入PCB209定量内标物工作液
(1.00mg/L)100μL,振荡混匀。加入25mL正己烷-二氯甲烷溶液,40℃水浴振荡提取1h,振荡速度
为200r/min。转移提取液至100mL鸡心瓶中。残渣中再加入20mL正己烷-二氯甲烷溶液,重复水
浴振荡提取1h。合并所有提取液,40℃水浴旋转蒸发浓缩至近干。
5.3.2 快速溶剂萃取(适用于单层食品接触用纸和复合食品接触用纸)
称取约2g(精确至0.01g)样品,加入PCB209定量内标物工作液(1.00mg/L)100μL后,与4g硅藻
土拌匀,装入底部放有玻璃纤维素滤纸片的不锈钢萃取池中(装样前萃取池底部先装入一层约2g的硅藻
土),再装入硅藻土充满不锈钢萃取池,拧上盖子,放置快速溶剂萃取仪萃取池托盘上进行萃取。快速溶剂萃取条件见表1。萃取完成后,将萃取液转入100mL鸡心瓶中,40℃水浴旋转蒸发浓缩至近干。
5.4 净化
吸取3mL正己烷超声洗涤鸡心瓶,洗涤液转移至15mL带刻度离心管中,40℃水浴氮吹浓缩至
约1mL,用正己烷定容为2.00mL,再加入3mL水,涡旋振荡30s,以5000r/min的转速离心5min。
吸取上清液至干净的15mL离心管中,加入1mL浓硫酸,涡旋振荡30s,以5000r/min的转速离心
5min。吸取上清液至干净的15mL离心管中,加入3mL水,涡旋振荡30s,以5000r/min的转速离
心5min。吸取上清液上机测定。
5.5 测定
5.5.1 气相色谱参考条件
a) 色谱柱:5%苯基-甲基聚硅烷填料毛细管柱,柱长30m,内径0.25mm,膜厚0.25μm。
b) 进样口温度:280℃。
c) 升温程序:开始温度90℃;以15℃/min升温至200℃,保持5min;以2.5℃/min升温至
250℃,保持2min;以20℃/min升温至290℃,保持5min。
d) 检测器温度:300℃。
e) 载气:高纯氮气(纯度≥99.999%),1.0mL/min。
f) 进样量:不分流模式,1.0μL。
在仪器最佳工作条件下,对待测溶液进样。标准系列溶液和试样溶液中被测物的响应值应在仪器
检测的线性范围内。色谱峰保留时间定性,内标法定量,必要时采用气相色谱-质谱法进行确证。8种
多氯联苯的标准溶液的气相色谱图参见图B.1。除不加试样外,采用完全相同的分析步骤、试剂和用
量,进行试剂空白试验。
6 分析结果的表述
试样中8种多氯联苯的含量按式(1)计算:
7 精密度
在重复性条件下获得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
PCB153和PCB180)的定量限均为0.010mg/kg。
9 原理
单层食品接触用纸中的多氯联苯采用正己烷-二氯甲烷混合溶液水浴振荡提取或快速溶剂萃取仪
提取;复合食品接触用纸中的多氯联苯采用快速溶剂萃取仪提取。提取液经浓缩,浓硫酸磺化处理后,
用气相色谱-质谱仪进行检测,内标法定量。
10 试剂和材料
除非另有说明,本方法所用试剂均为分析纯,水为GB/T 6682规定的一级水。
GB 31604.39-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Polychlorobiphenyls
(PCBs) in Food Contact Paper
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of 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
Foreword ... 3
1 Scope .. 4
2 Principle ... 4
3 Reagents and Materials .. 4
4 Instruments and Equipment .. 6
5 Analytical Procedures ... 6
6 Expression of Analytical Results ... 8
7 Precision ... 8
8 Others ... 8
9 Principle ... 9
10 Reagents and Materials ... 9
11 Instrument and Equipment ... 10
12 Analytical Procedures .. 10
13 Expression of Analytical Results ... 12
14 Precision ... 12
15 Others ... 12
Appendix A Relevant Information on 8 PCBs and Internal Standard Substance
... 13
Appendix B Gas Chromatogram of 8 PCBs and Internal Standard Substance
Standard Solution ... 14
Appendix C Characteristic Ions of 8 PCBs and Internal Standard Substance 15
Appendix D Gas Chromatography-Mass Spectrometry Total Ion
Chromatogram of 8 PCBs and Internal Standard Substance Standard Solution
... 16
Foreword
This Standard replaces SN/T 2200-2008 Food Contact Materials – Pulp, Paper and
Board – Determination of 7 Specified Polychlorinated Biphenyls (PCBs).
Compared with SN/T 2200-2008, this Standard has the major changes as follows.
--- Modify the standard name into “National Food Safety Standard – Food Contact
Materials and Articles – Determination of Polychlorobiphenyls (PCBs) in Food
Contact Paper”.
--- Increase the determination types of polychlorobiphenyls (increase PCB 118).
--- Modify the pre-treatment procedures.
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Polychlorobiphenyls
(PCBs) in Food Contact Paper
1 Scope
This Standard specifies using the gas chromatography and gas chromatography-mass
spectrometry to determine the polychlorobiphenyls in food contact paper.
This Standard’s first method is gas chromatography, the second method is gas
chromatography-mass spectrometry; both of which are applicable to determine 8
polychlorobiphenyls in the various food contact papers.
The First Method of Gas Chromatography
2 Principle
Polychlorobiphenyls (PCBs) in monolayer food contact paper are extracted through
water-bath shaking of n-hexane-dichloromethane mixed solution or extracted by
accelerated solvent extractor; polychlorobiphenyls (PCBs) in composite food contact
papers are extracted by accelerated solvent extractor. After the extracting solution is
concentrated, through the concentrated sulfuric acid solution treatment, it shall be
detected by the gas chromatograph equipped with electronic capture detector; use
internal standard method to quantify.
3 Reagents and Materials
Unless otherwise is specified, the reagents used in this method are analytically pure;
while the water is Class-I water stipulated in GB/T 6682.
3.1 Reagents
3.1.1 N-hexane (C6H14). chromatographic pure.
3.1.2 Dichloromethane (CH2Cl2).
3.1.4 Concentrated sulfuric acid (H2SO4). guarantee reagent.
3.2 Reagents preparation
3.2.1 N-hexane-dichloromethane mixed solution (1+1). weigh 100mL of n-hexane
and 100mL of dichloromethane; mxi evenly.
3.3 Standard substance
2, 2’, 5-trichlorobiphenyl (PCB18); 2, 4, 4’- trichlorobiphenyl (PCB 28); 2, 2’, 5, 5’-
tetrachlorobiphenyl (PCB 52); 2, 2’, 4, 5, 5’-pentachlorobiphenyl (PCB 101); 2, 3’, 4, 4’,
5- pentachlorobiphenyl (PCB 118); 2, 2’, 3, 4, 4’, 5’-hexachlorobiphenyl (PCB 138); 2,
2’, 4, 4’, 5, 5’- hexachlorobiphenyl (PCB 153); 2, 2’, 3, 4, 4’, 5, 5’-heptachlorobiphenyl
(PCB 209). purity of all standard substances is ≥98%; or the standard substances that
are approved by the state or awarded standard substance certificate by the state.
Relevant information on the 8 polychlorobiphenyls (PCBs) and internal standard
substance can refer to Table A.1.
3.4 Preparation of standard solution
3.4.1 PCBs and internal standard substance standard stock solution. accurately
weigh appropriate amount of PCBs standard substances; use n-hexane to prepare into
the solution with concentration of 200mg/L, respectively; seal and store at -18°C; the
shelf life is 12 months.
standard stock solutions; use n-hexane to gradually dilute into the 1.00mg/L mixed
standard working solution; seal and store at -18°C; the shelf life is 3 months.
3.4.3 Internal standard substance working solution. accurately pipette appropriate
amount of internal standard substance (PCB 209) standard stock solution; use n-
hexane to prepare into the solution with concentration of 1.00mg/L; seal and store at -
18°C; the shelf life is 3 months.
3.4.4 Mixed standard series solution. pipette appropriate amount of mixed standard
working solution and internal standard substance working solution; use n-hexane to
prepare into the mixed standard series solutions (the concentration of internal standard
0.050mg/L, 0.100mg/L and 0.200mg/L. It shall be prepared for current use.
3.5 Materials
3.5.1 Nylon filter. 0.22µm.
3.5.2 Diatomaceous earth carrier G. excellent grade; CAS No. of 68855-54-9; heat
for 4h in the 400°C muffle furnace before use, then prepare for later-use.
The Second Method of Gas Chromatography – Mass Spectrometry
9 Principle
Polychlorobiphenyls (PCBs) in monolayer food contact paper are extracted through
water-bath shaking by adopting the n-hexane-dichloromethane mixed solution or
food contact papers are extracted by accelerated solvent extractor. After the extracting
solution is concentrated, through the concentrated sulfuric acid solution treatment, it
shall be detected by the gas chromatograph-mass spectrometry; use internal standard
method to quantify.
10 Reagents and Materials
Unless otherwise is specified, the reagents used in this method shall be analytically
pure; while the water is Class-I water stipulated in GB/T 6682.
10.1 Reagents
10.1.1 N-hexane (C6H14). chromatographic pure.
10.1.3 Acetonitrile (C6H14) [here translator notes it shall be (CH3CN)].
chromatographic pure.
10.1.4 Concentrated sulfuric acid (H2SO4). guarantee reagent.
10.2 Preparation of specimen
10.2.1 N-hexane-dichloromethane mixed solution (1+1, volume ratio). weigh 100mL
of n-hexane and 100mL of dichloromethane, mix evenly.
10.3 Standard substance
2, 2’, 5-trichlorobiphenyl (PCB 18); 2, 4, 4’-trichlorobiphenyl (PCB 28), 2, 2’, 5, 5’-
tetrachlorobiphenyl (PCB52); 2, 2’, 4, 5, 5’-pentachlorobiphenyl (PCB 101); 2, 3’, 4, 4’,
2’, 4, 4’, 5, 5’-hexachlorobiphenyl (PCB 153); 2, 2’, 3, 4, 4’, 5, 5’-heptachlorobiphenyl
(PCB 180); internal standard substance (13C12-PCB 209). the purity of all standard
substances is ≥98%, or the standard substances approved by the state or awarded
standard substance certificate by the state; relevant information on 8 PCBs and
internal standard substance can refer to Table A.1.
10.4 Preparation of standard solution
The operation is the same as 5.1.
12.2 Preparation of specimen
The operation is the same as 5.2.
12.3.1 Water bath oscillation extraction (applicable to the monolayer food
contact paper)
Take about 2g (accurate to 0.01g) of sample into 50mL stopper glass centrifuge tube;
after adding 100µL of 13C12-PCB209 internal standard substance working solution
(1.00mg/L), the following operation is the same as 5.3.1.
12.3.2 Accelerated solvent extraction (applicable to the monolayer food
contact paper and composite food contact paper)
Take about 2g (accurate to 0.01g) of sample; after adding 100µL of 13C12-PCB209
internal standard substance working solution (1.00mg/L), the following operation is the
12.4 Purification
The operation is the same as 5.4.
12.5 Determination
12.5.1 Reference conditions of gas chromatography-mass spectrometry
a) Chromatographic column. 5% phenyl-methyl polysilane packing capillary column;
column length is 30m, inner diameter is 0.25mm, film thickness is 0.25µm.
b) Inlet temperature. 280°C.
c) Temperature-rise procedures. the starting temperature is 90°C; it rises to 200°C
at 15°C/min, maintain for 5min; then rise to 250°C at 2.5°C/min, maintain for
d) Ion source temperature. 230°C.
e) Ion source voltage. 70 eV.
f) Carrier gas. high-purity nitrogen (purity≥99.999%), 1.0mL/min.
g) injecting volume. splitless mode, 1.0µL.
h) The characteristic ions of 8 PCBs and the internal standard substance (13C12-
PCB209) can refer to Table C.1.
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