標準編號:	GB 31604.50-2020
中文名稱:	食品安全國家標準 食品接觸材料及制品 壬基酚遷移量的測定
英文名稱:	National food safety standard - Food contact materials and articles - Determination of nonylphenol migration
中標分類:	X09    衛生、安全、勞動保護
行業分類:	GB    國家標準
發布機構:	國家衛生健康委員會 國家市場監督管理總局
發布日期:	2020-09-11
實施日期:	2021-3-11
標準狀態:	valid
翻譯語言:	英文
文件格式:	PDF
中文字符數:	7000 字
翻譯價格(元):	420.0
交付時間:	付款后 1 個工作日

Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative. National food safety standard Food contact materials and articles Determination of nonylphenol migration 1 Scope This standard specifies the determination of nonylphenol migration in food contact materials and articles by liquid chromatography-mass spectrometry/mass spectrometry method. This standard is applicable to the determination of nonylphenol in soaking solution obtained by migration test on food contact materials and articles which use water, 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution, 50% (volume fraction) ethanol solution, olive oil and 95% (volume fraction) ethanol solution as food simulants respectively or use 95% (volume fraction) ethanol solution and isooctane chemical alternative solvent. 2 Principle For 4% (volume fraction) acetic acid solution as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on 4% (volume fraction) acetic acid and neutralized with ammonia water; for olive oil as food simulant, determination is carried out on the sample from the soaking solution obtained by migration test on olive oil and extracted with acetonitrile and purified with n-hexane; for isooctane as chemical alternative solvent, determination is carried out on the sample from the soaking solution obtained by migration test on isooctane and evaporated to dryness, then redissolved with methanol; for other solutions or chemical alternative solvent, determination is directly carried out on the soaking solutions obtained by migration test. The nonylphenol in soaking solution is determined by liquid chromatography-mass spectrometry/mass spectrometry method and quantified by external standard method. 3 Reagents and materials Unless otherwise specified, analytically-pure reagents and Class-I water specified in GB/T 6682 are adopted for the purpose of this method. 3.1 Reagents 3.1.1 Glacial acetic acid (C2H4O2). 3.1.2 Anhydrous ethanol (C2H6O). 3.1.3 95% ethanol. 3.1.4 Isooctane (C8H18). 3.1.5 Olive oil: chemically pure, complying with GB 5009.156. 3.1.6 Methanol (CH4O): chromatographically pure. 3.1.7 Acetonitrile (C2H3N): chromatographically pure. 3.1.8 N-hexane (C6H14). 3.1.9 Ammonia water: chromatographic purity, with a volume fraction ≥25%. 3.2 Preparation of reagents 4% (volume fraction) acetic acid solution, 10% (volume fraction) ethanol solution, 20% (volume fraction) ethanol solution and 50% (volume fraction) ethanol solution are prepared according to GB 5009.156. 3.3 Standards Nonylphenol (mixture of branched isomers, C15H24O, CAS No.: 84852-15-3) standard solution: 1,000mg/L 3.4 Preparation of standard solutions 3.4.1 Standard intermediate solution (100mg/L) Accurately transfer 1.00mL nonylphenol standard solution (1,000mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well. The solution is valid for 6 months in the refrigerator at 0℃~4℃. 3.4.2 Standard intermediate solution (5mg/L) Accurately transfer 0.50mL nonylphenol standard intermediate solution (100mg/L) into a 10mL volumetric flask, dilute to the scale with methanol, and then mix well. 3.4.3 Standard working solutions 3.4.3.1 4% (volume fraction) acetic acid standard working solution Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, and dilute to the scale with 4% (volume fraction) acetic acid solution. The standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L are obtained. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.1. 3.4.3.2 Oil-based food simulant standard working solution Accurately weigh 5.00g (accurate to 0.1mg) olive oil into six glass centrifuge tubes with stoppers respectively, add 0.01mL, 0.02mL, 0.03mL, 0.05mL, 0.10mL and 0.20mL standard intermediate solutions (5mg/L) respectively, vortex for mixing well to obtain 0.01mg/kg, 0.02mg/kg, 0.03mg/kg, 0.05mg/kg, 0.10mg/kg and 0.20mg/kg standard working solutions. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.2. 3.4.3.3 Isooctane standard working solution Accurately transfer 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with isooctane, and mix well to obtain the standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively. Prior to practice, the solutions shall be treated synchronously with food simulant soaking solution according to 5.1.2.3. 3.4.3.4 Other food simulant and chemical alternative solvent standard working solutions Accurately pipet 0.02mL, 0.04mL, 0.06mL, 0.10mL, 0.20mL and 0.40mL standard intermediate solutions (5mg/L) into six 10mL volumetric flasks respectively, dilute to the scale with corresponding food simulant or chemical alternative solvent to obtain other water-based food simulant or chemical alternative solvent standard working solutions with mass concentrations of 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.05mg/L, 0.10mg/L and 0.20mg/L respectively. 4 Apparatus 4.1 Liquid chromatography-tandem triple quadrupole mass spectrometer: equipped with electrospray ionization (ESI). 4.2 Vortex oscillator. 4.3 Analytical balances: with sensibility of 0.0001g and 0.01g respectively. 4.4 High-speed centrifuge: with a maximum rotation speed ≥10,000r/min. 5 Analysis steps 5.1 Preparation of test solution 5.1.1 Migration test Food contact materials and articles are subjected to migration test according to the requirements of GB 31604.1 and GB 5009.156. The soaking solution obtained by migration test shall be stored in a refrigerator at 4℃ free from light if cannot be tested immediately. The soaking solution shall be restored to room temperature before the next test. 5.1.2 Treatment of soaking solution 5.1.2.1 Treatment of 4% (volume fraction) acetic acid soaking solution Transfer 5.0mL 4% (volume fraction) acetic acid soaking solution obtained by migration test, add 0.5mL ammonia water, mix well, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined. 5.1.2.2 Treatment of oil-based food simulants Weigh 5.00g (accurate to 0.01g) olive oil soaking solution obtained by migration test into a glass centrifuge tube with stopper, add 2mL n-hexane, mix well, then add 5.0mL acetonitrile, vortex for oscillating for 0.5min, centrifuge for 5min at 4,000r/min, take the upper acetonitrile solution for centrifuging at 10,000r/min for 5min, and the supernatant is to be determined. 5.1.2.3 Treatment of isooctane soaking solution Transfer 10.0mL isooctane soaking solution obtained by migration test, evaporate to nearly dry at 40℃ in a rotary way, accurately transfer 10.0mL dissolved methanol residue, centrifuge for 5min at 10,000r/min , and the supernatant is to be determined. 5.1.2.4 Treatment of other food simulant soaking solutions and chemical alternative solvent soaking solutions Transfer a proper amount of soaking solution obtained by migration test, centrifuge for 5min at 10,000r/min, and the supernatant is to be determined. 5.1.3 Preparation of blank test solution Treat the food simulants and chemical alternative solvents that are not in contact with food contact materials and articles according to 5.1.1 and 5.1.2. 5.2 Instrument reference conditions 5.2.1 Liquid chromatography conditions The liquid chromatography reference conditions are as follows: a) Chromatographic column: C18 column, 2.6μm, 2.1mm×150mm (or equivalent). b) Mobile phase: methanol-water (90+10, volume ratio). c) Flow rate: 0.3mL/min. d) Column temperature: 40℃. e) Injection volume: 2μL. 5.2.2 Mass spectrometry conditions The mass spectrometry reference conditions are as follows: a) Ionization mode: electrospray ionization in negative ion mode (ESI-). b) Scanning mode of mass spectrometry: multi-reaction monitoring (MRM). c) See Table A.1 for other mass spectrometry parameters. 5.3 Plotting of standard curve Determine the standard working solution according to the instrument reference conditions listed in 5.2, plot the standard curve with the concentration of nonylphenol in the standard working solution as X-coordinate and the corresponding quantitative ion peak area as Y-coordinate, and obtain the linear equation. See Annex B for the chromatogram of nonylphenol standard working solution.

1 Scope 2 Principle 3 Reagents and materials 4 Apparatus 5 Analysis steps 6 Expression of analysis results 7 Precision 8 Others Annex A Reference mass spectrometry conditions Annex B MRM chromatogram of nonylphenol standard working solution

中華人民共和國國家標準 GB 31604.50—2020 食品安全國家標準 食品接觸材料及制品 壬基酚遷移量的測定 2020-09-11發布 2021-03-11實施 中華人民共和國國家衛生健康委員會 國家市場監督管理總局 發布 食品安全國家標準 食品接觸材料及制品 壬基酚遷移量的測定 1 范圍 本標準規定了食品接觸材料及制品壬基酚遷移量的液相色譜質譜/質譜測定方法。 本標準適用于食品接觸材料及制品以水、4％(體積分數)乙酸溶液、10％(體積分數)乙醇溶液、20％(體積分數)乙醇溶液、50％(體積分數)乙醇溶液、橄欖油、95％(體積分數)乙醇溶液為食品模擬物或采用95％(體積分數)乙醇溶液、異辛烷化學替代溶劑經遷移試驗所得浸泡液中壬基酚的測定。 2 原理 以4％(體積分數)乙酸溶液為食品模擬物經遷移試驗所得浸泡液加氨水中和后進樣測定；以橄欖油為食品模擬物經遷移試驗所得浸泡液經乙腈萃取和正己烷凈化后進樣測定；以異辛烷為化學替代溶劑經遷移試驗所得浸泡液蒸干后用甲醇復溶，進樣測定；其他遷移試驗所得浸泡液、化學替代溶劑浸泡液直接進樣測定。浸泡液中的壬基酚采用液相色譜質譜/質譜法測定，外標法定量。 3試劑和材料 除非另有說明，本方法所用試劑均為分析純，水為GB/T 6682規定的一級水。 3.1 試劑 3.1.1 冰乙酸(C2H4O2)。 3.1.2無水乙醇(C2H6O)。 3.1.3 95%乙醇。 3.1.4異辛烷(C8H18)。 3.1.5橄欖油：化學純，符合GB 5009.156的要求。 3.1.6 甲醇(CH4O)：色譜純。 3.1.7 乙腈(C2H3N)：色譜純。 3.1.8正己烷(C6H14)。 3.1.9氨水：色譜純，體積分數≥25％。 3.2 試劑配制 4％(體積分數)乙酸溶液、10％(體積分數)乙醇溶液、20％(體積分數)乙醇溶液、50％(體積分數)乙醇溶液的配制按GB 5009.156操作。 3.3 標準品 壬基酚(支鏈異構體的混合物，C15H24O，CAS號：84852-15-3)標準溶液：1 000 mg/L。 3.4標準溶液配制 3.4.1標準中間液(100 mg/L) 準確移取壬基酚標準溶液(1 000 mg/L)1.00 mL于10 mL容量瓶中，用甲醇稀釋并定容至刻度，混勻。此溶液在0℃～4℃冰箱中保存，有效期為6個月。 3.4.2標準中間液(5 mg/L) 準確移取壬基酚標準中間液(100 mg/L)0.50 mL于10 mL容量瓶中，用甲醇稀釋并定容至刻度，混勻。 3.4.3標準工作溶液 3.4.3.1 4％(體積分數)乙酸標準工作溶液 分別準確移取標準中間液(5 mg/L)0.02 mL、0.04 mL、0.06 mL、0.10 mL、0.20 mL、0.40 mL于6個10 mL容量瓶中，用4％(體積分數)乙酸溶液定容至刻度。得到質量濃度分別為0.01 mg/L、0.02 mg/L、0.03 mg/L、0.05 mg/L、0.10 mg/L、0.20 mg/L標準工作溶液。上機前需按照5.1.2.1與食品模擬物浸泡液同步處理。 3.4.3.2 油基食品模擬物標準工作溶液 分別準確稱取5.00 g(精確到0.1 mg)橄欖油于6個具塞玻璃離心管中，分別加入標準中間液(5 mg/L)0.01 mL、0.02 mL、0.03 mL、0.05 mL、0.10 mL、0.20 mL，渦旋混勻，得到分別為0.01 mg/kg、0.02 mg/kg、0.03 mg/kg、0.05 mg/kg、0.10 mg/kg、0.20 mg/kg標準工作溶液。上機前需按照5.1.2.2與食品模擬物浸泡液同步處理。 3.4.3.3異辛烷標準工作溶液 分別準確移取標準中間液(5 mg/L)0.02 mL、0.04 mL、0.06 mL、0.10 mL、0.20 mL、0.40 mL于6個10 mL容量瓶中，用異辛烷定容至刻度，混勻，得到質量濃度分別為0.01 mg/L、0.02 mg/L、0.03 mg/L、0.05 mg/L、0.10 mg/L、0.20 mg/L標準工作溶液。上機前需按照5.1.2.3與食品模擬物浸泡液同步處理。 3.4.3.4 其他食品模擬物、化學替代溶劑標準工作溶液 分別吸取標準中間液(5 mg/L)0.02 mL、0.04 mL、0.06 mL、0.10 mL、0.20 mL、0.40 mL于6個10 mL容量瓶中，用相應的食品模擬物或化學替代溶劑定容至刻度，得到質量濃度分別為0.01 mg/L、0.02 mg/L、0.03 mg/L、0.05 mg/L、0.10 mg/L、0.20 mg/L的其他水基食品模擬物或化學替代溶劑標準工作溶液。 4儀器和設備 4.1 液相色譜串聯三重四極桿質譜儀：配電噴霧離子源(ESI)。 4.2渦旋振蕩器。 4.3分析天平：感量0.000 1 g、0.01 g。 4.4高速離心機：最高轉速>10 000 r/min。 5分析步驟 5.1試液的制備 5.1.1 遷移試驗 食品接觸材料及制品按照GB 31604.1和GB 5009.156的要求進行遷移試驗。遷移試驗所得浸泡液如不能立即測試，應置于4℃冰箱中避光保存。若進行下一步試驗，應將浸泡液恢復至室溫后使用。 5.1.2浸泡液的處理 5.1.2.1 4％(體積分數)乙酸浸泡液的處理 移取遷移試驗所得4％(體積分數)乙酸浸泡液5.0 mL，加入0.5 mL氨水混勻后，經10 000 r/min離心5 min后，上清液待測。 5.1.2.2 油基食品模擬物的處理 稱取5.00 g(精確至0.01 g)遷移試驗所得橄欖油浸泡液至具塞玻璃離心管中，加入2 mL正己烷混勻，再加入5.0 mL乙腈，渦旋振蕩0.5 min，4 000 r/min離心5 min，取上層乙腈溶液經10 000 r/min離心5 min，上清液待測。 5.1.2.3異辛烷浸泡液的處理 移取遷移試驗所得異辛烷浸泡液10.0 mL，于40℃旋蒸至近干，準確移取10.0 mL甲醇溶解殘渣，經10 000 r/min離心5 min，上清液待測。 5.1.2.4 其他食品模擬物浸泡液、化學替代溶劑浸泡液的處理 移取適量遷移試驗所得浸泡液，經10 000 r/min離心5 min，上清液待測。 5.1.3 空白試液的制備 按5.1.1和5.1.2處理未與食品接觸材料及制品接觸的食品模擬物、化學替代溶劑。 5.2儀器參考條件 5.2.1 液相色譜條件 液相色譜參考條件如下： a)色譜柱：C18柱，2.6 μm，2.1 mm×150 mm(或等效色譜柱)。 b)流動相：甲醇-水(90+10，體積比)。 c)流速：0.3 mL/min。 d)柱溫：40℃。 e)進樣量：2μL。 5.2.2 質譜條件 質譜參考條件如下： a)離子化模式：電噴霧電離負離子模式(ESI)。 b)質譜掃描模式：多反應監測(MRM)。 c)其他質譜參數參見附錄A中表A.1。 5.3標準曲線的繪制 按照5.2所列的儀器參考條件，對標準工作溶液進行測定，以標準工作溶液中壬基酚的濃度為橫坐標，以對應的定量離子峰面積為縱坐標，繪制標準曲線，得到線性方程。壬基酚標準工作溶液的色譜圖參見附錄B。 5.4試液的測定 5.4.1 定性測定 按照5.2所列的儀器參考條件，測定食品模擬物試液和標準工作溶液，若試液與標準溶液中待測物的質量色譜峰保留時間的偏差在±2.5％范圍內；所有定性離子的信噪比均超過3：1，且定性離子對的相對豐度與濃度相當的標準溶液的相對豐度一致，相對豐度偏差不超過表1的規定，則可判斷樣品中存在相應的待測物。 表1 定性測定時相對離子豐度的最大允許偏差 相對離子豐度，k/％ k≥50 20