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食品新标准应对｜食品中N-亚硝胺化合物测定(GB 5009.26-2023)

来源：岛津（上海）实验器材有限公司分类：操作使用 2024-03-27 14:45:03 14阅读次数

- 引言 -

硝酸盐广泛存在于食品之中，很容易与胺化合生成亚硝胺。亚硝胺与苯并芘、黄曲霉素是世界公认的三大强致癌物质。

长期小剂量食用含亚硝胺的食品就可以使人致癌。随着人们健康意识的逐步提高，对食品品质要求越来越高，对于食品中的N-亚硝胺类化合物污染问题也越来越受到关注。

本文参考GB 5009.26-2023《食品安全国家标准食品中N-亚硝胺类化合物的测定》第二法（QuEChERS-气相色谱-质谱/质谱法），使用岛津GCMS-TQ8040 NX三重四极杆气质联用仪，结合PTV程序升温进样技术，建立了测定食品中NDMA含量的方法。此方法的优点是前处理简单快速，灵敏度高，结果准确，可为食品中NDMA含量测定提供参考。

文末附应用报告下载链接

1. 仪器和分析条件

GCMS-TQ8040 NX三重四极杆气质联用仪+ PTV-2030程序升温进样口

色谱柱：

SH-Wax，30 m×0.25 mm×0.50 μm

柱温程序：40℃(0.5min)_15℃/min_190℃_25℃/min_240℃(5 min)

PTV进样口温度：50℃(0.5min)_400℃/min_220℃(5 min)

PTV放空时间：0.16 min

离子源温度：250℃

载气控制：恒流模式，1 mL/min

接口温度：250℃

进样方式：不分流进样

检测器电压：调谐电压+0.6 kV

进样量：5 μL

采集方式：MRM，见表1

2. 样品前处理

图1 样品前处理流程图

提取盐包：

380-00147-03, SHIMSEN QuEChERS Extraction Salts, 4g MgSO4, 1g NaCl for NDMA in Food, 50/P

净化管：

380-00147-04, SHIMSEN QuEChERS dSPE, 15mL, 150mg PLS-A for NDMA in Food, 50/P

除水管：

380-00147-07, SHIMSEN QuEChERS dSPE, 15mL, 1.6g MgSO4, 0.4g NaCl for NDMA in Food, 50/P

3. 实验结果

3.1 标准样品的色谱图

图2 NDMA及内标物的质量色谱图

表1 NDMA 及对应内标物保留时间及MRM 参数

3.2 重复性实验

对浓度为0.5 μg/L 的NDMA 标准溶液连续进样6 次，考察重复性。NDMA 峰面积RSD 为2.82%，重复性良好。

表2 NDMA 重复性

3.3 回收率

各称取腊肉、腊鱼空白样品5 g，称取牛肉空白样品10 g，添加一定浓度的NDMA，每种基质加标样品平行处理1 份，样品的加标回收率结果见表3。

表3 回收率实验结果

4. 结论

采用GCMS-TQ8040 NX 三重四极杆气相色谱质谱联用仪，结合PTV 程序升温进样技术，参考国家标准，使用SH-Wax气相色谱柱，QuEChERS前处理方法。建立了测定食品中NDMA 含量的方法。

在方法定量限的加标浓度下，NDMA 的回收率分布在84.64~100.22% 之间。

此方法定量准确、灵敏度高，可为食品中NDMA 的准确测定提供参考。

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[8]未定义数组索引: page
[2]Declaration of app\common\model\TechNewsCategory::getList($filter = Array) should be compatible with app\common\model\BaseModel::getList($filter = Array, $sort = Array)
[8]未定义数组下标: 0
[2]Declaration of app\common\model\TechNews::getAllList($filter = Array, $limit = 10, $order = Array, $with = Array) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\Company::getAllList($filter = Array, $limit = 20) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
[8]Only variables should be passed by reference
[2]Declaration of app\common\model\TechNewsComment::getAllList($filter = Array, $limit = 16) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8192]Function create_function() is deprecated
[8192]Function create_function() is deprecated
[8]未定义数组索引: area
[8]未定义数组索引: st
[2]Declaration of app\common\model\Topic::getList($filter = Array) should be compatible with app\common\model\BaseModel::getList($filter = Array, $sort = Array)
[2]Declaration of app\common\model\Topic::getAllList($filter = Array, $field = 'id,md5,tit...', $limit = 0) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\TopicInfoList::getAllList($filter = Array, $limit = 8) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\News::getAllList($filter = Array, $limit = 16, $order = Array, $with = Array) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[8]未定义数组索引: center
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
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[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: goods_list
[8]未定义数组下标: 0
[8]未定义数组索引: center
[8]未定义数组索引: center
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[ SQL ] SELECT `id` FROM `user_follow` WHERE `user_id` IS NULL AND `follow_user_id` = 203 LIMIT 1 [ RunTime:0.000213s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_comment` [ RunTime:0.000729s ]
[ SQL ] SELECT * FROM `tech_news_comment` WHERE `tech_news_id` = 3086 AND `parent_id` = 0 ORDER BY `id` DESC [ RunTime:0.000211s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `tech_news_comment` WHERE `tech_news_id` = 3086 LIMIT 1 [ RunTime:0.000159s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `is_show` = 1 AND `review_status` = 1 AND `id` IN (3086,3287,3217,3133,3098,3059,2760,2471,1815,1716) ORDER BY field(id,3086,3287,3217,3133,3098,3059,2760,2471,1815,1716) [ RunTime:0.000531s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (203,197,474,452,306,714,245,297,316,240) [ RunTime:0.001144s ]
[ SQL ] SHOW COLUMNS FROM `topic` [ RunTime:0.001061s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `topic` WHERE `review_status` = 1 ORDER BY `id` DESC LIMIT 4 [ RunTime:0.000186s ]
[ SQL ] SHOW COLUMNS FROM `topic_info_list` [ RunTime:0.001024s ]
[ SQL ] SELECT * FROM `topic_info_list` WHERE `topic_id` = 1 ORDER BY `id` DESC LIMIT 2 [ RunTime:0.000351s ]
[ SQL ] SHOW COLUMNS FROM `news` [ RunTime:0.001004s ]
[ SQL ] SELECT * FROM `news` WHERE `id` IN (864,849) [ RunTime:0.000260s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `tech_news` WHERE `review_status` = 1 AND `is_show` = 1 ORDER BY `id` DESC LIMIT 10 [ RunTime:0.000232s ]
[ SQL ] SHOW COLUMNS FROM `user` [ RunTime:0.000787s ]
[ SQL ] SELECT `a`.* FROM `user` `a` INNER JOIN `tech_news` `b` ON `a`.`id`=`b`.`user_id` GROUP BY `a`.`id` ORDER BY `b`.`id` DESC LIMIT 10 [ RunTime:0.007693s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (592,413,444,224,13,239,598,697,394,285) [ RunTime:0.001259s ]
[ SQL ] SHOW COLUMNS FROM `seo` [ RunTime:0.000801s ]
[ SQL ] SELECT * FROM `seo` WHERE `column_type` = '16' AND `page_type` = 'tech_news' AND `info_id` = 3086 LIMIT 1 [ RunTime:0.000211s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3086 [ RunTime:0.001127s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3287 [ RunTime:0.000915s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3217 [ RunTime:0.000879s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3133 [ RunTime:0.001536s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3098 [ RunTime:0.001528s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3059 [ RunTime:0.000919s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2760 [ RunTime:0.000868s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 2471 [ RunTime:0.000874s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1815 [ RunTime:0.000871s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1716 [ RunTime:0.000887s ]
[ SQL ] SELECT * FROM `user` WHERE `id` = 203 LIMIT 1 [ RunTime:0.000156s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 592 LIMIT 1 [ RunTime:0.000161s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 592 LIMIT 1 [ RunTime:0.000196s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 413 LIMIT 1 [ RunTime:0.000148s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 413 LIMIT 1 [ RunTime:0.000119s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 444 LIMIT 1 [ RunTime:0.000118s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 444 LIMIT 1 [ RunTime:0.000134s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 224 LIMIT 1 [ RunTime:0.000124s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 224 LIMIT 1 [ RunTime:0.000114s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 13 LIMIT 1 [ RunTime:0.000113s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 13 LIMIT 1 [ RunTime:0.000110s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 239 LIMIT 1 [ RunTime:0.000112s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 239 LIMIT 1 [ RunTime:0.000118s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 598 LIMIT 1 [ RunTime:0.000114s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 598 LIMIT 1 [ RunTime:0.000110s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 697 LIMIT 1 [ RunTime:0.000111s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 697 LIMIT 1 [ RunTime:0.000114s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 394 LIMIT 1 [ RunTime:0.000130s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 394 LIMIT 1 [ RunTime:0.000116s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 285 LIMIT 1 [ RunTime:0.000111s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 285 LIMIT 1 [ RunTime:0.000109s ]

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