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食品安全国家标准 食品接触材料及制品 软木中杂酚油的测定
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GB 31604.36-2016
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标准编号: GB 31604.36-2016 (GB31604.36-2016)
中文名称: 品安全国家标准 食品接触材料及制品 软木中杂酚油的测定
英文名称: Food contact materials for export -- Wood materials -- Determination of cresol in cork -- Gas chromatography-mass spectrometry method
行业: 国家标准
中标分类: X09
字数估计: 10,179
发布日期: 2016-10-19
实施日期: 2017-04-19
旧标准 (被替代): SN/T 2828-2011
标准依据: 国家卫生和计划生育委员会公告2016年第15号
GB 31604.36-2016: 食品安全国家标准 食品接触材料及制品 软木中杂酚油的测定
GB 31604.36-2016 英文名称: Food contact materials for export -- Wood materials -- Determination of cresol in cork -- Gas chromatography-mass spectrometry method
１ 范围
本标准规定了食品接触材料软木中杂酚油的气相色谱-质谱测定方法。
本标准适用于食品接触材料软木中杂酚油的测定。
２ 原理
试样中的杂酚油用无水乙醇在索氏（Ｓｏｘｈｌｅｔ）抽提器中进行提取，浓缩提取液并定容。提取液用０．４５μｍ有机系微孔滤膜过滤后，用气相色谱-质谱联用仪（ＧＣ-ＭＳ）测定，以保留时间定性，外标法定量。
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
无水乙醇（ＣＨ３ＣＨ２ＯＨ）。
３．２ 标准品
杂酚油标准品：纯度均不低于９８％，见附录Ａ。
３．３ 标准溶液的配制
３．３．１ 标准储备液的配制
分别准确称取适量的杂酚油标准品，用无水乙醇配制成浓度为１００μｇ／ｍＬ的标准储备液。
３．３．２ 标准工作液的配制
取标准储备液，用无水乙醇逐级稀释成浓度为０．０１μｇ／ｍＬ、０．０２μｇ／ｍＬ、０．０５μｇ／ｍＬ、０．１μｇ／ｍＬ、０．２μｇ／ｍＬ的标准工作液，或根据需要配制成适用浓度的标准工作液。
注：标准储备液在０～４℃冰箱中保存有效期６个月。
４ 仪器和设备
４．１ 气相色谱-质谱联用仪。
４．２ 索氏抽提器：１５０ｍＬ。
４．３ 旋转蒸发器。
４．４ 切割研磨机。
４．５ 有机系微孔滤膜：孔径０．４５μｍ。
５ 分析步骤
５．１ 试样制备
取适量软木样品，用切割研磨机将样品切割并研磨成粒径不超过１ｍｍ的粉末，充分混匀并贮存于
密闭容器中，避光保存。
５．２ 试样的提取
准确称取２ｇ（精确至１ｍｇ）试样于１５０ｍＬ索氏抽提器的纸筒中，在圆底烧瓶中加入８０ｍＬ无水乙醇，８０℃～９５℃进行４ｈ提取，１ｈ内回流次数不少于４次。冷却后，用旋转蒸发器５０℃旋转蒸发，直到剩下约５ｍＬ，用无水乙醇转移定容至１０ｍＬ，试液经有机系滤膜过滤后，待气相色谱-质谱测定。
５．３ 测定
５．３．１ 仪器参考条件
５．３．１．１ 气相色谱-质谱参考条件
以下参数可供参考，具体实例可参见附录Ｂ。
ａ） 色谱柱：石英毛细管柱；
ｂ） 载气：Ｈｅ，纯度为≥９９．９９９％；
ｃ） 程序升温；
ｄ） 进样方式：不分流进样；
ｅ） 离子化方式：ＥＩ；
ｆ） 电子能量：７０ｅＶ；
ｇ） 测定方式：选择离子监测（ＳＩＭ）。
５．３．１．２ 气相色谱-质谱检测及确证
进行样品测定时，如果检出的色谱峰的保留时间与标准样品相一致，并且在扣除背景后的样品质谱
图中，所选离子均出现，并且其丰度比与标准品的丰度比值在允许范围内（允许范围见表１），则可判定样品中存在相应的目标物。
注：在上述气相色谱-质谱条件下，９种杂酚油标准物的气相色谱-质谱选择离子色谱图参见附录Ｂ。
５．３．２ 标准曲线的制作
将标准系列工作液分别注入气相色谱-质谱联用仪，测定相应的峰高或峰面积。以标准工作液的浓
度为横坐标，以峰面积为纵坐标，绘制标准曲线。
６ 分析结果的表述
样品中每种杂酚油的含量按式（１）计算。
７ 精密度
在重复性条件下，获得两次独立测试结果的绝对差值不得超过算术平均值的１０％。
８ 其他
当取样量２．００ｇ，定容至１０．００ｍＬ时，定量限均为０．５ｍｇ／ｋｇ。
GB 31604.36-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -
Food contact materials and products -
Determination of creosote in cork
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 . 5
5 Analytical steps . 5
6 Expression of the analytic result .. 6
7 Precision. 7
8 Others . 7
Appendix A Names, CAS number, chemical structure formula and molecular
formula of 9 kinds of creosote compounds .. 8
Appendix B Examples for determination of 9 kinds of creosote compounds .. 10
Foreword
This standard replaces SN/T 2828-2011 "Food contact materials for export.
Wood materials. Determination of cresol in cork. Gas chromatography-mass
spectrometry method".
Compared with SN/T 2828-2011, the main differences of this standard are as
follows.
- Changed the name of the standard to "National Food Safety Standard -
Food contact materials and products -Determination of creosote in cork";
- Replaced single point method to standard curve method for quantitative
method.
National Food Safety Standard -
Food contact materials and products -
Determination of creosote in cork
1 Scope
This standard specifies the gas chromatography-mass spectrometry method for
the determination of creosote in cork for food contact materials.
This standard is applicable to the determination of creosote in cork for food
contact materials.
2 Principle
Extract the creosote in the sample by Soxhlet extractor with absolute ethyl
alcohol, concentrate the extracted solution and the meter volume. Filter the
extracted solution by 0.45μm organic microporous membrane, then determine
by gas chromatography-mass spectrometry (GC-MS). Use retention time for
qualitative determination and external standard method for quantitative
determination.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method all shall be analytical
pure. The water shall be the primary water specified in GB/T 6682.
3.1 Reagents
Absolute ethyl alcohol (CH3CH2OH).
3.2 Standard substance
Standard creosote. purity no less than 98%, see appendix A.
3.3 Preparation of standard solutions
3.3.1 Preparation of standard reserve solution
Prepare the standard reserve solution 100 μg/mL with absolute ethyl alcohol.
3.3.2 Preparation of standard working solution
Dilute the standard reserve solution into 0.01μg/mL, 0.02μg/mL, 0.05μg/mL,
0.1μg/mL and 0.2μg/mL of standard working solution with absolute ethyl alcohol.
Or make standard working solution with suitable concentration as required.
Note. The valid period for standard solution stored in 0~4°C refrigerator is 6 months.
4 Instruments and equipment
4.1 Gas chromatography-mass spectrometry.
4.2 Soxhlet extractor. 150mL.
4.3 Rotary evaporator.
4.4 Cutting grinder.
4.5 Organic microporous membrane. pore diameter 0.45μm.
5.1 Sample preparation
Take appropriate amount of cork sample, cut and ground into powder with
diameter less than 1mm by cutting and grinding machine, fully mix and store in
a closed container avoiding light.
5.2 Sample extraction
Weigh accurately 2g of sample (accuracy to 1mg), put in the cylinder of 150mL
Soxhlet extractor and add 80mL of absolute ethyl alcohol into round-bottom
flask. Exact at 80°C and 95°C for 4 hours with the reflux no less than 4 times in
1 hour. After cooling, evaporate with rotating evaporator at 50°C until about 5
Filter by organic filter membrane and wait for determination by gas
chromatography-mass spectrometry (GC-MS).
5.3 Determination
5.3.1 Instrument reference condition
5.3.1.1 Gas chromatography-mass spectrometry reference condition
The following parameters are available for reference, see Appendix B for
example.
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