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食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
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GB 31604.35-2016
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标准编号: GB 31604.35-2016 (GB31604.35-2016) 中文名称: 食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定 英文名称: Determination of perfluorooctane sulfonates (PFOS) in the food packaging materials -- High performance liquid chromatography-tandem mass spectrometry 行业: 国家标准 中标分类: X09 字数估计: 8,821 发布日期: 2016-10-19 实施日期: 2017-04-19 旧标准 (被替代): GB/T 23243-2009 标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.35-2016: 食品安全国家标准 食品接触材料及制品 全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的测定
GB 31604.35-2016 英文名称: Determination of perfluorooctane sulfonates (PFOS) in the food packaging materials -- High performance liquid chromatography-tandem mass spectrometry
1 范围
本标准规定了食品接触材料及制品中全氟辛烷磺酸(PFOS)和全氟辛酸(PFOA)的液相色谱-串联质谱测定方法。
本标准适用于纸板盒类、橡胶类、聚乙烯类、塑料类、树脂类、不粘锅涂层等食品接触材料及制品中
PFOS和PFOA的测定。
2 原理
食品接触材料及制品中的PFOS和PFOA采用甲醇作为提取溶剂,加速溶剂萃取法提取,弱阴离
子交换固相萃取柱净化,液相色谱分离,电喷雾离子源(ESI)电离,多反应监测模式(MRM)检测,同位素内标法定量。
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。
注:本标准中使用到的所有有机溶剂和材料,在使用前,应进行空白实验。如本底值高于定量限,应对有机溶剂进行重蒸,更换试验材料,直至本底值低于定量限。
3.1 试剂
3.1.1 甲醇(CH3OH):色谱纯。
3.1.2 乙腈(CH3CN):色谱纯。
3.1.3 乙酸铵(CH3COONH4):优级纯。
3.1.4 冰乙酸(CH3COOH)。
3.1.5 氨水(NH3·H2O)。
3.2 试剂配制
称取0.385g乙酸铵,用水溶解并定容至1000mL,摇匀,过0.22μm滤膜。
3.2.2 0.1%氨化甲醇取200mL甲醇于250mL容量瓶内,准确移取250μL氨水于甲醇中,甲醇定容,超声混匀。
取0.385g乙酸铵,用180mL水溶解,加冰乙酸调节pH至4±0.5,用水定容至200mL。
3.3 标准品
3.3.1 全氟辛烷磺酸(PFOS)(C8HF17O3S,CAS号:1763-23-1),纯度≥99%,或经国家认证并授予标准物质证书的标准物质。
3.3.2 全氟辛酸(PFOA)[CF3(CF2)6COOH,CAS号:335-67-1],纯度≥98%,或经国家认证并授予标准物质证书的标准物质。
3.3.3 1,2,3,4-13C4-PFOS(MPFOS)和13C4-PFOA(MPFOA)标准品溶液:浓度均为50μg/mL。
3.4 标准溶液配制
3.4.1 PFOS和PFOA混合标准储备溶液
准确称取PFOS和PFOA各5mg(精确至0.00001g),用甲醇稀释定容至100mL容量瓶,配制成浓度均为50μg/mL的PFOS和PFOA标准溶液。-4℃环境下保存。
3.4.2 PFOS和PFOA混合标准工作溶液
吸取PFOS和PFOA标准溶液,用甲醇稀释,配制成PFOS和PFOA浓度分别为100ng/mL的混合标准工作溶液。-4℃环境下保存。
3.4.3 同位素内标混合工作溶液
吸取MPFOS和MPFOA混合标准储备溶液,用甲醇稀释,配制成MPFOS和MPFOA浓度为100ng/mL的同位素内标混合工作溶液。-4℃环境下保存。
3.4.4 PFOS、PFOA和同位素内标混合标准工作溶液
用甲醇稀释PFOS、PFOA混合标准工作液和同位素内标混合工作溶液,配制PFOS和PFOA浓度为2ng/mL、5ng/mL、10ng/mL、20ng/mL和40ng/mL的系列PFOS、PFOA和同位素内标(内标浓度均为2ng/mL)混合工作溶液。-4℃环境下保存。
3.5 材料
3.5.1 微孔滤膜:有机系,孔径0.22μm。
3.5.2 弱阴离子交换(WeakAnionExchanger,WAX)固相萃取柱:150mg/6mL。
3.5.3 液氮。
4 仪器和设备
注:为降低高效液相色谱管道中引入的PFOS和PFOA的污染,需要对特氟龙材质管路替换为PEEK管路或不锈钢管路。
4.1 液相色谱-串联质谱仪:配有电喷雾离子源(ESI)。
4.2 天平:感量为0.01mg。
4.3 加速溶剂萃取仪。
4.4 涡旋振荡器。
4.5 氮吹仪。
4.6 冷冻研磨机。
5 分析步骤
5.1 试样制备
塑料类、硅胶类试样:剪碎至5mm ×5mm 以下,再用液氮冷冻粉碎机研磨成粉末状;树脂类打
碎,再用液氮冷冻粉碎机研磨成粉末状;涂层类试样:用小刀刮下,再用液氮冷冻粉碎机研磨成粉末状;
纸板盒类、聚乙烯类试样:用剪刀剪成1cm ×1cm大小。
5.2 提取和净化
5.2.1 提取
称取1g(精确至0.01g)试样,放入加速溶剂萃取池中,提取溶剂为甲醇,提取溶剂体积为60%的样品池体积,萃取温度为110℃,加热时间5min,平衡5min,重复2次,萃取液放置至室温,氮气吹干至约0.5mL,加10mL水,混匀待净化。
5.2.2 净化
依次用4mL0.1%氨化甲醇、4mL甲醇、4mL水活化平衡 WAX固相萃取柱后,将上述溶液转移至固相萃取柱内,加4mL25mmol/L乙酸铵缓冲液淋洗,4mL0.1%氨化甲醇洗脱,收集洗脱液于40℃下氮气吹干,1mL甲醇复溶后过0.22μm微孔滤膜,LC-MS/MS分析。
5.3 液相色谱参考条件
5.3.1 色谱柱:C18,柱长150mm,内径2.1mm,粒径3μm,或同等性能色谱柱。
5.3.2 柱温:40℃。
5.3.3 进样量:10μL。5.3.4 流动相:5mmol/L乙酸铵:乙腈,梯度洗脱条件见表1。
5.3.5 流速:0.2mL/min。
5.4 质谱参考条件
5.4.1 离子源:电喷雾离子源(ESI)。
5.4.2 扫描极性:负离子扫描。
5.4.3 扫描方式:多反应监测(MRM)。
GB 31604.35-2016
5.4.4 电喷雾电压:-4000V。
5.4.5 鞘气(N2)温度:325℃。
5.4.6 鞘气流速:12.0L/min。
5.4.7 干燥气温度:250℃。
5.4.8 干燥气流速:10.0L/min。
5.4.9 监测离子对信息、碰撞能量等见表2。
5.5 定性测定
按上述条件测定试样和标准工作溶液,如果试样的质量色谱峰保留时间与标准物质一致,允许偏差
为±2.5%;定性离子对的相对丰度与浓度相当的标准工作溶液的相对丰度一致,相对丰度允许偏差不超过表3规定的范围,则可判断样品中存在相应的被测物。
GB 31604.35-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Food contact materials and products -
Determination of perfluorooctane sulfonate (PFOS) and
perfluoro caprylic acid (PFOA)
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 . 7
6 Expression of the analytic result .. 9
7 Precision. 10
8 Others .. 10
Appendix A Chromatogram . 11
Foreword
This standard replaces GB/T 23243-2009 "Determination of perfluorooctane
sulfonates (PFOS) in the food packaging material - High performance liquid
chromatography-tandem mass spectrometry".
The main technical differences of this standard in comparison with GB/T 23243-
2009 are as follows.
- Changed the name of the standard to read "National Food Safety Standard
- Food contact materials and products - Determination of perfluorooctane
sulfonate (PFOS) and perfluoro caprylic acid (PFOA)";
- Added scope of application of the standard;
- Added the content of determination object PFOA;
- Added the method of sample preparation;
- Added the purification step. Use the weak anion exchange solid phase
extraction column to purify;
- Increased the sensitivity of the determination method.
National Food Safety Standard -
Food contact materials and products -
Determination of perfluorooctane sulfonate (PFOS) and
perfluoro caprylic acid (PFOA)
1 Scope
This standard specifies the method for the determination of perfluorooctane
sulfonate (PFOS) and perfluorooctanoic acid (PFOAA) in food contact materials
and products by tandem mass spectrometry.
This standard is applicable to the determination of PFOS and PFOA in food
contact materials and products such as carton, rubber, polyethylene, plastics,
resin, non-stick pan coating and so on.
2 Principle
PFOS and PFOA in food contact materials and products were extracted by
methanol to accelerate solvent extraction, purified by weak anion exchange
solid-phase extraction column, separated by liquid chromatography, ionized by
electrospray ionization, determined by multi-reaction monitoring mode and
quantified by Isotopic internal standard quantity.
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.
Note. All organic solvents and materials used in this standard shall be blank tested before using. If the
background value is higher than the quantitative limit, the organic solvent shall be re-steamed. Replace
the test material until the background value is below the limit of quantification.
3.1 Reagents
3.1.1 Methanol (CH3OH). Chromatographic purity.
3.1.2 Acetonitrile (CH3CN). Chromatographic purity.
5 Analytical steps
5.1 Sample preparation
For plastics, silica gel sample. cut to size below 5mm×5mm; then grind into
powder by liquid nitrogen frozen grinder. For resin. smash then grind into
powder with liquid nitrogen frozen grinder. For coated sample. scrape with knife,
then grind into powder by liquid nitrogen frozen grinder. For cardboard box and
5.2 Extraction and purification
5.2.1 Extraction
Weigh 1g (accurate to 0.01g) of sample and put it into an accelerated solvent
extraction pool. The extraction solvent is methanol. The volume of extraction
solvent is 60% the volume of the sample pool. The extraction temperature shall
be 110°C. The heating time shall be 5 min. Balance for 5 min. Repeat twice.
Place the extraction solution at room temperature. Dry with nitrogen-blowing to
about 0.5 mL. Add 10mL of water and mix for purification.
5.2.2 Purification
methanol animation, 4 mL of methanol and 4 mL of water in turn. Then transfer
the above solution to the solid phase extraction column. Add 4mL of 25mmol/L
ammonium acetate buffer solution to rinse-wash. Add 4 mL of 0.1% ammonia
methanol to elute. Collect the eluent and dry by nitrogen at 40°C. Re-dissolve
by 1 mL of methanol, then pour through.22μm microporous membrane. Analyze
by LC- MS/MS.
5.3 Reference conditions for liquid chromatography
5.3.1 Chromatographic column. C18, column length is 150mm, inner diameter
is 2.1mm, particle size is 3μm, or the column with equivalent performance.
5.3.3 Sample volume. 10μL.
5.3.4 Mobile phase. 5 mmol/L ammonium acetate. acetonitrile. For gradient
elution conditions, see Table 1.
5.3.5 Flow rate. 0.2 mL/min.
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