GB/T 44364-2024 牙膏中丙烯酰胺的测定 高效液相色谱串联质谱法

ICS

71.100.40

CCS

Y43

中华人民共和国国家标准

GB/T44364—2024

牙膏中丙烯酰胺的测定高效液相色谱

串联质谱法

Determinationofacrylamideintoothpaste—

Highperformanceliquidchromatographytandemmassspectrometry

2024-08-23发布2025-03-01实施

国家市场监督管理总局

发布

国家标准化管理委员会

GB/T44364—2024

目次

前言

Ⅲ

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1

范围

1

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2

规范性引用文件

1

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3

术语和定义

1

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4

原理

1

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5

试剂和材料

1

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6

仪器设备

2

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7

试验步骤

2

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7.1

试样溶液的制备

2

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7.2

测定

2

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7.3

标准工作曲线绘制

3

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7.4

试样测定

3

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7.5

空白试验

4

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8

结果计算

4

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9

回收率

4

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10

精密度

4

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11

检测限和定量限

4

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附录A（资料性）

丙烯酰胺标准物质/标准样品及内标信息

5

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附录B（资料性）

丙烯酰胺及其内标标准溶液的多反应监测色谱图

6

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Ⅰ

GB/T44364—2024

前言

本文件按照GB/T1.1—2020《标准化工作导则第1部分：标准化文件的结构和起草规则》的规

定起草。

请注意本文件的某些内容可能涉及专利。本文件的发布机构不承担识别专利的责任。

本文件由中国轻工业联合会提出。

本文件由全国口腔护理用品标准化技术委员会（SAC/TC492）归口。

本文件起草单位：苏州世谱检测技术有限公司、苏科世谱生物技术（苏州）有限公司、苏州质量检

测科学研究院、苏州市科耐瑞检测技术有限公司、广州舒客实业有限公司、广州质量监督检测研究院、

黑龙江省轻工科学研究院、无限极（中国）有限公司、福建爱洁丽日化有限公司、柳州两面针股份有限

公司、重庆登康口腔护理用品股份有限公司、浙江方圆检测集团股份有限公司、河北省食品检验研究

院、江苏省产品质量监督检验研究院、江苏省食品药品监督检验研究院、完美（广东）日用品有限公

司、清华大学、深圳大学、海南大学、苏州大学、常州大学、常州市食品药品纤维质量监督检验中心、

苏州市药品检验检测研究中心、山东华素健康护理品有限公司。

本文件主要起草人：张岩、卢剑、方方、何霜、朱丹丹、郑卫、结莉、李建祥、刘斌、秦天依、

叶竹洪、刘文玉、陈敏珊、高艳、蔡丽萍、胡永志、张环、杨铭、肖俊芳、代丹、陈晓珍、郭新东、

王怡、黄金凤、张迎阳、黄志宁、宋淑文、聂炎炎、卢应红、姜雷、高龙、顾盼、刘群林、高红影、

朱钇蓉、唐文金。

Ⅲ

GB/T44364—2024

牙膏中丙烯酰胺的测定高效液相色谱

串联质谱法

警示─使用本文件的人员应有正规实验室工作的实践经验。本文件并未指出所有可能的安全问题。

使用者有责任采取适当的安全和健康措施，并保证符合国家有关规定的条件。

1范围

本文件描述了牙膏中丙烯酰胺的高效液相色谱串联质谱测定方法的原理、试剂和材料、仪器设备、

试验步骤、结果计算、回收率和精密度、允许差等内容。

本文件适用于牙膏中丙烯酰胺的测定。

2规范性引用文件

下列文件中的内容通过文中的规范性引用而构成本文件必不可少的条款。其中，注日期的引用文

件，仅该日期对应的版本适用于本文件；不注日期的引用文件，其最新版本（包括所有的修改单）适用

于本文件。

GB/T6682分析实验室用水规格和试验方法

3术语和定义

本文件没有需要界定的术语和定义。

4原理

牙膏中丙烯酰胺经水提取、正己烷净化后，采用高效液相色谱串联质谱仪多反应监测模式检测，以

保留时间和特征碎片离子丰度比定性，内标法定量。

5试剂和材料

5.1除另有说明，所用试剂均为色谱纯，水为符合GB/T6682要求的一级水。

5.2乙腈。

5.3正己烷。

5.4甲酸。

5.50.1%（体积分数）甲酸溶液：取1mL甲酸（5.4），用水稀释至1L，混合均匀。

5.6标准物质/标准样品：丙烯酰胺标准物质/标准样品的英文名称、CAS号、分子式、相对分子质量

和化学结构式见附录A中表A.1，纯度不小于98%。

13

5.7同位素内标：C﹘丙烯酰胺的英文名称、CAS号、分子式、相对分子质量和化学结构式见表A.1，

3

纯度不小于98%。

5.8标准储备液：准确称取丙烯酰胺标准物质/标准样品（5.6）10mg（精确至0.0001g）于10mL容

量瓶中，用乙腈（5.2）溶解并稀释至刻度，即得质量浓度为1000µg/mL的标准储备液。于2℃～8℃

避光保存，可保存12个月。

1