气相色谱质谱法测定日化用品中的卡拉花醛

doi:10.3969/j.issn.1001-1803.2020.08.011

日用化学工业 ›› 2020, Vol. 50 ›› Issue (8): 572-575.doi: 10.3969/j.issn.1001-1803.2020.08.011

气相色谱质谱法测定日化用品中的卡拉花醛

刘婷(),汤杭燕,朱丽萍,郭方龙,刘海山,严颖鹏

浙江省检验检疫科学技术研究院,浙江杭州 311215

收稿日期:2019-11-04 修回日期:2020-07-29 出版日期:2020-08-22 发布日期:2020-08-25
作者简介:刘婷（1984-）,女,浙江湖州人,高级工程师,硕士,电话：13958028944,E-mail： liuting1594@126.com。
基金资助:
原浙江出入境检验检疫局课题(ZK201715)

Determination of karanal in daily chemicals by GC-MS

LIU Ting(),TANG Hang-yan,ZHU Li-ping,GUO Fang-long,LIU Hai-shan,YAN Ying-peng

Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou, Zhejiang 311215, China

Received:2019-11-04 Revised:2020-07-29 Online:2020-08-22 Published:2020-08-25

摘要/Abstract

摘要：

建立了气相色谱质谱联用法测定日化用品中卡拉花醛,以甲醇为提取溶剂,超声提取,经膜过滤后,过滤液直接进行气相色谱质谱测定,外标法定量。结果表明,该方法最低定量限为0.5 μg/g,在0.05~10 mg/L的质量浓度范围内,峰面积和质量浓度呈现良好的线性关系,当添加水平分别为0.5,5和10 μg/g时,加标回收率为70.1% ~96.9%,方法精密度（RSD,n=6）为6.0%~6.8%。该方法适用范围广,可操作性强,简便快捷,准确可靠,可满足日化用品中卡拉花醛的测试需求。

关键词: 日化用品, 卡拉花醛, 气相色谱质谱法

Abstract:

A method for the determination of karanal in daily chemicals by gas chromatography mass spectrometry （GC-MS） was established. It was ultrasonically extracted by methanol as extraction solvent. After membrane filtration, the filtrate was directly determined by GC-MS, and quantitative by external standard method. The results show that the limit of quantity is 0.5 μg/g. In the range of 0.05-10 mg/L, there is a good linear relationship between the peak area and the mass concentration of karanal. The average recoveries at three spiked levels of 0.5, 5 and 10 μg/g change from 70.1% to 96.9%, and the precisions （RSD, n=6） vary from 6.0% to 6.8%. The method has the advantages of wide application, strong operability, simplicity, rapidity, accuracy and reliability, and can meet the testing requirements of karanal in daily chemical products.

Key words: daily chemicals, karanal, gas chromatography mass spectrometry

中图分类号:

TQ658

刘婷,汤杭燕,朱丽萍,郭方龙,刘海山,严颖鹏. 气相色谱质谱法测定日化用品中的卡拉花醛[J]. 日用化学工业, 2020, 50(8): 572-575.

LIU Ting,TANG Hang-yan,ZHU Li-ping,GUO Fang-long,LIU Hai-shan,YAN Ying-peng. Determination of karanal in daily chemicals by GC-MS[J]. China Surfactant Detergent & Cosmetics, 2020, 50(8): 572-575.

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参考文献 8

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[4]	Wang Jing, Li Ju, Yu Jianlong, at al. Determination of karanal and its isomers in detergents by gas chromatography-mass spectrometry[J]. Journal of Instrumental Analysis, 2017,36(9) : 1104-1108.
[5]	Wang Chengyun, Huang Jian, Yang Zuojun, et al. Rapid determination of karanal in paper products[J]. Paper Science ＆ Technology, 2018,37(2) : 73-75,78.
[6]	Wang Chengyun, Wang Gang, Liu Yi. Rapid determination of karanal in paper products by ultra-high performance liquid chromatography[J]. China Pulp & Paper Industry, 2018,39(8) : 20-23.
[7]	Wang Chengyun, Zhang Yushuang, Cui Wei, et al. Determination of karanal in textiles by HPLC[J]. Melliand China, 2018,46(3) : 52-56.
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序号	温度/℃	t/min	峰面积	w/（μg·g^-1）
1	室温（25）	10	4 523 662	5.85
2	室温（25）	10	4 930 768	6.43
3	室温（25）	20	4 416 651	5.69
4	室温（25）	20	4 651 808	6.03
5	45	10	4 645 921	6.02
6	45	10	4 529 142	5.85
7	45	20	5 033 227	6.58
8	45	20	4 555 334	5.89

序号	添加水平/（μg·g^-1）	测试结果/（μg·g^-1）	回收率/ %	相对标准偏差/ %
1	0.5	0.43	85.5	6.6
2		0.40	79.6
3		0.43	85.9
4		0.45	90.3
5		0.48	96.9
6		0.44	87.0
7	5	4.63	92.6	6.0
8		4.03	80.5
9		4.10	82.0
10		4.08	81.7
11		4.49	89.8
12		4.48	89.6
13	10	8.25	82.5	6.8
14		8.20	82.0
15		7.01	70.1
16		7.51	75.1
17		7.13	71.3
18		7.77	77.7

气相色谱质谱法测定日化用品中的卡拉花醛

Determination of karanal in daily chemicals by GC-MS

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