GB/T 44364-2024牙膏中丙烯酰胺的測(cè)定高效液相色譜串聯(lián)質(zhì)譜法

ICS

71.100.40

CCS

Y43

中華人民共和國(guó)國(guó)家標(biāo)準(zhǔn)

GB/T44364—2024

牙膏中丙烯酰胺的測(cè)定高效液相色譜

串聯(lián)質(zhì)譜法

Determinationofacrylamideintoothpaste—

Highperformanceliquidchromatographytandemmassspectrometry

2024-08-23發(fā)布2025-03-01實(shí)施

國(guó)家市場(chǎng)監(jiān)督管理總局發(fā)布

國(guó)家標(biāo)準(zhǔn)化管理委員會(huì)

GB/T44364—2024

目次

前言

·····································································································

Ⅲ

1

范圍

··································································································

1

2

規(guī)范性引用文件

······················································································

1

3

術(shù)語(yǔ)和定義

···························································································

1

4

原理

··································································································

1

5

試劑和材料

···························································································

1

6

儀器設(shè)備

······························································································

2

7

試驗(yàn)步驟

······························································································

2

7.1

試樣溶液的制備

·················································································

2

7.2

測(cè)定

······························································································

2

7.3

標(biāo)準(zhǔn)工作曲線繪制

···············································································

3

7.4

試樣測(cè)定

·························································································

3

7.5

空白試驗(yàn)

·························································································

4

8

結(jié)果計(jì)算

······························································································

4

9

回收率

································································································

4

10

精密度

·······························································································

4

11

檢測(cè)限和定量限

·····················································································

4

附錄A（資料性）

丙烯酰胺標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品及內(nèi)標(biāo)信息

··········································

5

附錄B（資料性）

丙烯酰胺及其內(nèi)標(biāo)標(biāo)準(zhǔn)溶液的多反應(yīng)監(jiān)測(cè)色譜圖

·································

6

Ⅰ

GB/T44364—2024

前言

本文件按照GB/T1.1—2020《標(biāo)準(zhǔn)化工作導(dǎo)則第1部分：標(biāo)準(zhǔn)化文件的結(jié)構(gòu)和起草規(guī)則》的規(guī)

定起草。

請(qǐng)注意本文件的某些內(nèi)容可能涉及專利。本文件的發(fā)布機(jī)構(gòu)不承擔(dān)識(shí)別專利的責(zé)任。

本文件由中國(guó)輕工業(yè)聯(lián)合會(huì)提出。

本文件由全國(guó)口腔護(hù)理用品標(biāo)準(zhǔn)化技術(shù)委員會(huì)（SAC/TC492）歸口。

本文件起草單位：蘇州世譜檢測(cè)技術(shù)有限公司、蘇科世譜生物技術(shù)（蘇州）有限公司、蘇州質(zhì)量檢

測(cè)科學(xué)研究院、蘇州市科耐瑞檢測(cè)技術(shù)有限公司、廣州舒客實(shí)業(yè)有限公司、廣州質(zhì)量監(jiān)督檢測(cè)研究院、

黑龍江省輕工科學(xué)研究院、無(wú)限極（中國(guó)）有限公司、福建愛潔麗日化有限公司、柳州兩面針股份有限

公司、重慶登康口腔護(hù)理用品股份有限公司、浙江方圓檢測(cè)集團(tuán)股份有限公司、河北省食品檢驗(yàn)研究

院、江蘇省產(chǎn)品質(zhì)量監(jiān)督檢驗(yàn)研究院、江蘇省食品藥品監(jiān)督檢驗(yàn)研究院、完美（廣東）日用品有限公

司、清華大學(xué)、深圳大學(xué)、海南大學(xué)、蘇州大學(xué)、常州大學(xué)、常州市食品藥品纖維質(zhì)量監(jiān)督檢驗(yàn)中心、

蘇州市藥品檢驗(yàn)檢測(cè)研究中心、山東華素健康護(hù)理品有限公司。

本文件主要起草人：張巖、盧劍、方方、何霜、朱丹丹、鄭衛(wèi)、結(jié)莉、李建祥、劉斌、秦天依、

葉竹洪、劉文玉、陳敏珊、高艷、蔡麗萍、胡永志、張環(huán)、楊銘、肖俊芳、代丹、陳曉珍、郭新東、

王怡、黃金鳳、張迎陽(yáng)、黃志寧、宋淑文、聶炎炎、盧應(yīng)紅、姜雷、高龍、顧盼、劉群林、高紅影、

朱釔蓉、唐文金。

Ⅲ

GB/T44364—2024

牙膏中丙烯酰胺的測(cè)定高效液相色譜

串聯(lián)質(zhì)譜法

警示─使用本文件的人員應(yīng)有正規(guī)實(shí)驗(yàn)室工作的實(shí)踐經(jīng)驗(yàn)。本文件并未指出所有可能的安全問(wèn)題。

使用者有責(zé)任采取適當(dāng)?shù)陌踩徒】荡胧?，并保證符合國(guó)家有關(guān)規(guī)定的條件。

1范圍

本文件描述了牙膏中丙烯酰胺的高效液相色譜串聯(lián)質(zhì)譜測(cè)定方法的原理、試劑和材料、儀器設(shè)備、

試驗(yàn)步驟、結(jié)果計(jì)算、回收率和精密度、允許差等內(nèi)容。

本文件適用于牙膏中丙烯酰胺的測(cè)定。

2規(guī)范性引用文件

下列文件中的內(nèi)容通過(guò)文中的規(guī)范性引用而構(gòu)成本文件必不可少的條款。其中，注日期的引用文

件，僅該日期對(duì)應(yīng)的版本適用于本文件；不注日期的引用文件，其最新版本（包括所有的修改單）適用

于本文件。

GB/T6682分析實(shí)驗(yàn)室用水規(guī)格和試驗(yàn)方法

3術(shù)語(yǔ)和定義

本文件沒有需要界定的術(shù)語(yǔ)和定義。

4原理

牙膏中丙烯酰胺經(jīng)水提取、正己烷凈化后，采用高效液相色譜串聯(lián)質(zhì)譜儀多反應(yīng)監(jiān)測(cè)模式檢測(cè)，以

保留時(shí)間和特征碎片離子豐度比定性，內(nèi)標(biāo)法定量。

5試劑和材料

5.1除另有說(shuō)明，所用試劑均為色譜純，水為符合GB/T6682要求的一級(jí)水。

5.2乙腈。

5.3正己烷。

5.4甲酸。

5.50.1%（體積分?jǐn)?shù)）甲酸溶液：取1mL甲酸（5.4），用水稀釋至1L，混合均勻。

5.6標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品：丙烯酰胺標(biāo)準(zhǔn)物質(zhì)/標(biāo)準(zhǔn)樣品的英文名稱、CAS號(hào)、分子式、相對(duì)分子質(zhì)量

和化學(xué)結(jié)構(gòu)式見附錄A中表A.1，純度不小于98%。

5.7同位素內(nèi)標(biāo)：13C3?丙烯酰胺的英文名稱、CAS號(hào)、分子式、相對(duì)分子質(zhì)量和化學(xué)結(jié)構(gòu)式見表A.1，

純度不小于98%。

5.8標(biāo)準(zhǔn)儲(chǔ)備液：準(zhǔn)確稱