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食品安全国家标准 食品接触材料及制品 塑料中环氧乙烷和环氧丙烷的测定
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GB 31604.27-2016
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标准编号: GB 31604.27-2016 (GB31604.27-2016)
中文名称: 食品安全国家标准 食品接触材料及制品 塑料中环氧乙烷和环氧丙烷的测定
英文名称: Food contact materials -- Determination of ethylene oxide and propylene oxide in plastics -- Gas chromatography
行业: 国家标准
中标分类: X09
字数估计: 12,163
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): GB/T 23296.11-2009
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.27-2016: 食品安全国家标准 食品接触材料及制品 塑料中环氧乙烷和环氧丙烷的测定
GB 31604.27-2016 英文名称: Food contact materials -- Determination of ethylene oxide and propylene oxide in plastics -- Gas chromatography
1 范围
本标准规定了食品接触材料及制品中环氧乙烷和环氧丙烷的测定方法。
本标准适用于塑料食品接触材料及制品中环氧乙烷和环氧丙烷的测定。
第一法 顶空气相色谱-质谱法
2 原理
样品中环氧乙烷或环氧丙烷经N,N-二甲基乙酰胺(DMAC)提取后,采用顶空进样,在色谱柱中环
氧乙烷或环氧丙烷与内标物乙醚及其他组分分离,用质谱检测器检测,以内标法定量。
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
N,N-二甲基乙酰胺(简称DMAC,C4H9NO,CAS号:127-19-5):色谱纯,色谱图上与环氧乙烷或
环氧丙烷有相同保留时间的杂质峰面积不得超过1%。
3.2 标准品
3.2.1 环氧乙烷(C2H4O,CAS号:75-21-8):纯度≥99%,或经国家认证并授予标准物质证书的标准
物质。
3.2.2 环氧丙烷(C3H6O,CAS号:200-879-2):纯度≥99%,或经国家认证并授予标准物质证书的标准
物质。
3.2.3 乙醚(C4H10O,CAS号:60-29-7):纯度≥99.5%,或经国家认证并授予标准物质证书的标准物
质。色谱图上与环氧乙烷或环氧丙烷有相同保留时间的杂质峰面积不得超过1%。
3.3 标准溶液配制
3.3.1 环氧乙烷标准储备液
称取50mg(精确到0.0001g)环氧乙烷,用DMAC溶解后,定容至50mL,配制成浓度为1mg/mL的
储备液。溶液在4℃下避光密封储存,有效期为2个月。
3.3.2 环氧丙烷标准储备液
称取50mg(精确到0.0001g)环氧丙烷,用DMAC溶解后,定容至50mL,配制成浓度为1mg/mL的
储备液。溶液储存条件同3.3.1。
3.3.3 环氧乙烷、环氧丙烷混标中间溶液
量取5mLDMAC于50mL容量瓶中,用刻度吸量管分别吸取2.0mL环氧乙烷标准储备液
(3.3.1)及1.0mL环氧丙烷标准储备液(3.3.2)于该容量瓶中,用DMAC定容,获得环氧乙烷、环氧丙烷
混标中间溶液。环氧乙烷、环氧丙烷浓度分别为40.0μg/mL、20.0μg/mL。溶液储存条件同3.3.1。
3.3.4 环氧乙烷、环氧丙烷混标溶液
用刻度吸量管分别吸取5.0mLDMAC于6个10mL容量瓶中,分别用微量注射器吸取25μL、
50μL、100μL、250μL、500μL、1000μL环氧乙烷、环氧丙烷混标中间溶液(3.3.3)加入上述6个容量
瓶中,用DMAC定容。获得环氧乙烷的浓度分别为0.1μg/mL、0.2μg/mL、0.4μg/mL、1.0μg/mL、
2.0μg/mL、4.0μg/mL,环氧丙烷的浓度分别为0.05μg/mL、0.1μg/mL、0.2μg/mL、0.5μg/mL、
1.0μg/mL、2.0μg/mL。溶液储存条件同3.3.1。
3.3.5 乙醚内标储备液
称取50mg(精确至0.0001g)乙醚于预先盛有5mLDMAC的50mL容量瓶中,用DMAC定容,
配制成浓度为1mg/mL的储备液。溶液储存条件同3.3.1。
3.3.6 乙醚内标中间溶液
量取5mLDMAC于10mL容量瓶中,再用刻度吸量管吸取2.5mL的乙醚内标储备液(3.3.5)于
该容量瓶中,用DMAC定容,获得乙醚内标中间溶液。其浓度为250.0μg/mL。溶液储存条件同3.3.1。
4 仪器和设备
4.1 气相色谱-质谱联用仪:配备电子轰击离子源(EI)和顶空自动进样器。
4.2 微量注射器:10μL、100μL、1000μL。
4.3 顶空瓶:20mL,配备铝盖和丁基橡胶或硅树脂橡胶隔垫,隔垫接触样品一面应涂有聚四氟乙烯。
4.4 分析天平:感量0.0001g。
4.5 机械振荡器。
5 分析步骤
5.1 试样处理
可溶于DMAC的试样直接称量;不溶于DMAC的试样,使用冷冻研磨仪或剪刀等切割工具将其破
碎成粒径小于1mm×1mm后,尽快称量。切割样品时,不可使其发热变软。
5.2 试样溶液的制备
称取1.0g±0.1g试样(5.1)于顶空瓶中,用刻度吸量管吸取5.0mLDMAC于顶空瓶中,用微量注
射器加入10μL的乙醚内标中间溶液(3.3.6)后,尽快用盖密封。对于可溶于DMAC的试样,用机械振
荡器以每两秒一次的频率振荡顶空瓶直至试样溶解;对于不溶于DMAC的试样,用机械振荡器以每两
秒一次的频率振荡顶空瓶4h。若样品浓度超出线性范围,可在加入内标溶液前用DMAC适当稀释,使
其浓度处于线性范围内。
5.3 空白溶液的制备
除不加试样外,采用与5.2完全相同的分析步骤、试剂和用量。
5.4 仪器参考条件
5.4.1 顶空进样器条件
顶空进样器条件列出如下:
a) 样品平衡时间:可溶于DMAC的样品为30min,不溶于DMAC的样品为60min;
b) 顶空瓶温度:100℃;
c) 定量环温度:105℃。
5.4.2 气相色谱条件
气相色谱条件列出如下:
a) 色谱柱:键合苯乙烯-二乙烯苯的PLOT柱,柱长30m,内径0.32mm,膜厚20μm;
b) 进样口温度:200℃;
c) 进样方式:分流进样,分流比为1∶1;
d) 柱温:60℃下恒温1min,以10℃/min升至100℃,以20℃/min升至180℃并恒温2min,
以30℃/min升至250℃并恒温4min;
e) 载气:氦气。
5.4.3 质谱条件
质谱条件列出如下:
a) 质谱接口温度:280℃;
b) 四级杆温度:150℃;
d) 电离能量:70eV;
e) 测定方式:选择离子监测模式,监测离子范围:m/z15~m/z100。环氧乙烷的特征离子为15、
29、43、44,其中44为定量离子;环氧丙烷的特征离子为28、31、43、58,其中58为定量离子;乙
醚的特征离子为31、45、59、74,其中74为定量离子。
5.5 标准曲线的制作
用刻度吸量管分别吸取5.0mL环氧乙烷、环氧丙烷混标溶液(3.3.4)于6个顶空瓶中,再用微量注
射器分别加入10μL乙醚内标中间溶液(3.3.6),尽快用盖密封。按照5.4所列测定条件,分别将上述溶
液依次通过顶空气相色谱-质谱仪测定。分别以溶液中环氧乙烷(或环氧丙烷)浓度为横座标,单位为微
克每毫升(μg/mL),以对应环氧乙烷(或环氧丙烷)峰面积与乙醚峰面积之比为纵座标,分别绘制标准
5.6 试样溶液的测定
将试样溶液和空白溶液注入顶空气相色谱-质谱仪测定,得到环氧乙烷(或环氧丙烷)与乙醚峰面积
之比,由标准曲线得到试样溶液中环氧乙烷(或环氧丙烷)的浓度。
GB 31604.27-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food contact
materials and products - Determination of ethylene
oxide and epoxy propane in plastics
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of People's
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Principle... 4
3 Reagents and materials ... 4
4 Instruments and equipment ... 6
5 Analytical steps ... 6
6 Expression of the analytic result ... 9
7 Precision... 10
8 Others ... 10
9 Principle... 10
10 Reagents and materials... 10
11 Instruments and equipment ... 12
12 Analytical steps ... 12
13 Expression of the analytic result ... 15
14 Precision ... 15
15 Others ... 16
Appendix A Standard chromatogram of ethylene oxide and epoxy propane 17
National Food Safety Standard - Food contact materials
and products - Determination of ethylene oxide and
epoxy propane in plastics
1 Scope
This standard specifies the methods of determination of ethylene oxide and
epoxy propane in food contact materials and products.
This standard is applicable to the determination of ethylene oxide and epoxy
propane in plastic food contact materials and products.
The first method -
Headspace gas chromatography-mass spectrometry
2 Principle
After ethylene oxide or epoxy propane being extracted by N, N-dimethyl
acetamide (DMAC), introduce it in the sample by headspace injection.
Separate the ethylene oxide or epoxy propane from the internal standard
diethyl ether and other components in the chromatographic column. Detect
with spectrum detector, determine the quantity by internal standard method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method shall be analytical
pure. The water shall be the primary water specified in GB/T 6682.
3.1 Reagents
N, N-dimethyl acetamide (DMAC, C4H9NO, CAS. 127-19 -5). color spectrum
pure. The area of the impurity peak with the same retention time of ethylene
oxide or epoxy propane shall not exceed 1%.
3.2 Standard product
3.2.1 Ethylene oxide (C2H4O, CAS. 75-21-8). purity ≥99%, or a standard
2.0μg/mL, 4.0μg/mL; the concentrations of epoxy propane are respectively
0.05μg/mL, 0.1μg/mL, 0.2μg/mL, 0.5μg/mL, 1.0μg/mL, 2.0μg/mL. The
storage condition of the solution is the same as 3.3.1.
3.3.5 Diethyl ether internal standard reserve solution
Weigh 50 mg (precision to 0.0001 g) of diethyl ether, put into a 50mL
volumetric flask containing 5mL of DMAC. Meter with DMAC and obtain the
reserve solution with concentration of 1 mg/mL. The storage condition of the
solution is the same as 3.3.1.
3.3.6 Diethyl ether internal standard intermediate solution
Weigh 5mL of DMAC and put into a 10mL volumetric flask, then draw with
graduated pipette 2.5mL of the diethyl ether internal standard reserve solution
(3.3.5) and put into the volumetric flask. Meter with DMAC and obtain the
diethyl ether internal standard intermediate solution. The concentration is
250.0μg/mL. The storage condition of the solution is the same as 3.3.1.
4 Instruments and equipment
4.1 Gas chromatography-mass spectrometer. equipped with electron
4.2 Micro-syringe. 10μL, 100μL, 1000μL;
4.3 Headspace bottle. 20mL, equipped with aluminum cap and butadiene
rubber or silicone rubber spacer. The spacer shall be coated with
polytetrafluoroethylene on the side contacting sample.
4.4 Analytical balance. sensitivity 0.0001g.
4.5 Mechanical oscillator.
5 Analytical steps
5.1 Sample treatment
The sample soluble in DMAC shall be weighed directly. The sample which is
1mm by cutting tools such as cryogenic grinder or scissors, and be weighed
as soon as possible. When cutting the sample, shall not make it heated and
soft.
5.2 Preparation of sample solution
e) Carrier gas. helium.
5.4.3 Mass spectrometry conditions
The mass spectrum conditions are as follows.
a) Mass spectrum interface temperature. 280°C;
b) Quadrupole rod temperature. 150°C;
d) Ionization energy. 70 eV;
e) Determination method. select ion monitoring mode, monitor ion range.
m/z 15 ~ m/z 100. The qualitative ions of ethylene oxide are 15, 29, 43,
44, of which 44 is quantitative ion; the qualitative ions of epoxy propane
are 28, 31, 43, 58, of which 58 is quantitative ion; the qualitative ions of
diethyl ether are 31, 45, 59, 74, of which 74 is quantitative ion.
5.5 Making of standard curve
Draw with graduated pipette 5.0 mL of ethylene oxide and epoxy propane
mixed standard solution (3.3.4) to 6 headspace bottles respectively. Add
of diethyl ether (3.3.6) and seal with cover as soon as possible. Under the
conditions provided in 5.4, put the above solutions respectively through
headspace gas chromatography-mass spectrometer to determine. Use the
concentrations of ethylene oxide (or epoxy propane) in the solution as
abscissa in unit of microgram per milliliter (μg/mL) and the peak area ratio of
ethylene oxide (or epoxy propane) to diethyl ether as ordinate to draw
standard curves respectively. See A.1 for standard chromatogram.
5.6 Determination of sample solution
Inject the sample solution and blank solution into the headspace gas
ethylene oxide (or epoxy propane) to diethyl ether. Obtain the concentration
of ethylene oxide (or epoxy propane) in sample solution from the standard
curve.
5.7 Qualitative
When determine the sample under the same experimental conditions, if the
deviation of the chromatographic peak retention time of the substance to be
determined in the sample solution is within ±2.5% of the chromatographic
peak retention time of the standard substance; and all the selected ions
10.2.1 Ethylene oxide (C2H4O, CAS. 75-21-8). purity ≥99%, or a standard
certificate.
10.2.2 Epoxy propane (C3H6O, CAS.200-879-2). purity ≥99%, or a standard
substance certified by the State and granted the standard substance
certificate.
10.2.3 Diethyl ether (C4H10O, CAS. 60-29-7). purity ≥99.5%, or a standard
substance certified by the State and granted the standard substance
certificate. The area of the impurity peak with the same retention time of
ethylene oxide or epoxy propane shall not exceed 1%.
10.3 Standard solution preparation
Weigh 50 mg (precision to 0.0001 g) of ethylene oxide, dissolve with DMAC,
meter the volume to 50 mL, obtain the reserve solution with concentration of
1mg/mL. Store the solution at 4°C sealed and keep away from light. The
validity period is 2 months.
10.3.2 Epoxy propane standard reserve solution
Weigh 50 mg (precision to 0.0001 g) of epoxy propane, dissolve with DMAC,
meter the volume to 50 mL, obtain the reserve solution with concentration of
1mg/mL. Store the solution at 4°C sealed and keep away from light. The
validity period is 2 months.
epoxy propane
Draw 5.0mL of DMAC and put into 6 10mL volumetric flasks respectively.
Draw with micro-syringe respectively 0μL, 40μL, 100μL, 200μL, 300μL,
400μL of the ethylene oxide standard reserve solution (10.3.1) and put into
the above-mentioned 6 volumetric flasks respectively. Draw with
micro-syringe 0μL, 40μL, 100μL, 200μL, 300μL, 400μL of the epoxy propane
standard reserve solution (10.3.2) and put into the above-mentioned 6
volumetric flasks respectively. Meter with DMAC to the scale. Thus, obtain the
mixed standard intermediate solution of ethylene oxide and epoxy propane.
10μg/mL, 20μg/mL, 30μg/mL, 40μg/mL; the concentrations of epoxy propane
are respectively 0μg/mL, 4μg/mL, 10μg/mL, 20μg/mL, 30μg/mL, 40μg/mL.
The storage condition of the solution is the same as 10.3.1.
10.3.4 Diethyl ether internal standard reserve solution
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