中国塑料 ›› 2019, Vol. 33 ›› Issue (10): 89-93.DOI: 10.19491/j.issn.1001-9278.2019.10.016

• 标准与测试 • 上一篇    下一篇

捕集肼自动顶空气相色谱法测定PET瓶装水中乙醛

黄焯枝,徐红,毛新   

  1. 达能(中国)食品饮料有限公司
  • 收稿日期:2019-05-13 修回日期:2019-06-24 出版日期:2019-10-26 发布日期:2019-10-25

Determination of Acetaldehyde in PET Bottled Water by Automatic Headspace-trap Gas Chromatography

HUANG Zhuozhi,XU Hong,MAO Xin   

  1. Danone(China)Food &Beverage CoLtdZhongshan 528415.China
  • Received:2019-05-13 Revised:2019-06-24 Online:2019-10-26 Published:2019-10-25
  • Contact: HUANG Zhuozhi E-mail:zhuozhi.huang@danone.com

摘要: 建立捕集肼自动顶空气相色谱法测定聚对苯二甲酸乙二醇酯(PET)瓶装水中乙醛含量的方法。取10 mL样品加入4 g氯化钠,样品通过捕集肼富集以提高灵敏度,自动顶空进样器炉温:80 ℃、取样针温度:130 ℃、传输线温度:135 ℃、炉温平衡时间:20 min;捕集肼吸附温度:30 ℃、解吸温度:280 ℃、循环次数:3;气相进样口温度:200 ℃、FID温度:200 ℃,采用HP-INNOWAX色谱柱及在50~100 ℃温度范围内程序升温进行分离,线性范围在50 μg/L内,检出限为5 μg/L,加入20 μg/L和50 μg/L标准溶液做加收率试验及精密度试验,测得平均回收率为92.9 %,相对标准偏差为2.08 %~4.01 %(n=6)。该方法操作简单、快速、灵敏度高、重现性好,可满足于PET瓶装水乙醛含量的检测。。

关键词: 捕集肼顶空-气相色谱法, 聚对苯二甲酸乙二醇酯, 瓶装水, 乙醛, 检出限

Abstract: This paper established a methodology for determining the content of acetaldehyde in the bottled water in PET bottles by automatic headspace-trap gas chromatography. This methodology includes the following steps: 10 mL of water sample was taken and then 4 g of sodium chloride was added into the sample. The sample was enriched by trap to improve sensitivity for gas chromatographic analysis. The temperature of headspace oven was set as 80 ℃, the needle temperature as 130 ℃, the transmission line temperature as 135 ℃, the balance time of oven as 20 min, the trap adsorption temperature as 30 ℃, the desorption temperature as 280 ℃, the cycle number as 3 times, the GC injection temperature as 200 ℃, and the FID temperature was set as 200 ℃. Moreover, the HP-INNOWAX column was used with the programmed temperature elevation in the temperature range of 50~100 ℃. Moreover, the linearity range was kept within 50 μg/L with a detection limit of 5 μg/L, and the recovery and precision were tested at two concentration levels of 20 μg/L and 50 μg/L. The average recovery was measured to be 92.9 % and RSD values were determined as 2.08 %~4.01 % with a correlation coefficient of 6. This method is simple, rapid, sensitive and reproducible and can be used for the determination of acetaldehyde in the bottled water.

Key words: automatic headspace-trap gas chromatography, polvethvlene terephthalate, bottled wa ter: acetaldehydedetection limit

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