线性不好？峰型拖尾？乳铁蛋白新标准无忧应对(GB 5009.299-2024)-医疗器械网

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线性不好？峰型拖尾？乳铁蛋白新标准无忧应对(GB 5009.299-2024)

来源：岛津（上海）实验器材有限公司分类：行业标准 2024-04-29 16:22:43 20阅读次数

乳铁蛋白新标准

(GB 5009.299-2024)

线性不好？峰型拖尾？

SGLC“柱”您一臂之力

日前，国家卫健委、市场监督局联合发布了《食品安全国家标准食品添加剂使用标准》（GB 2760-2024）等47项新标准和6项修改单^[1]。

其中，《食品安全国家标准食品中乳铁蛋白的测定发布》(GB 5009.299-2024)^[2]是首个适用于乳制品中牛乳铁蛋白含量的测定的国家标准，并将于2024年8月实施。

在实际样品中乳铁蛋白的测试过程中，往往会存在峰型拖尾、曲线线性不佳、回收率不稳定等问题。针对以上问题点，小编将为您带来SGLC的解决方案，“柱”您一臂之力，无忧应对新标准的方法开发。

文末附解决方案下载及产品试用！

01

样品前处理

采用SHIMSEN肝素亲和柱(3mg/3mL, PN: 380-00930-02) 进行样品处理。

乳粉样品平行测试5次，加标回收率86%，RSD1.8% (产品标识浓度62.33mg/100g，加标浓度40mg/100g，实测浓度88.07mg/100g)

实验操作及缓冲液配置请按照产品使用说明进行，参考步骤如下

前处理参考步骤——固态样品

!

前处理过程中的注意事项如下

1

缓冲液尽量现用现配，避免pH变化；

2

滤膜及样品瓶在使用前，应进行吸附测试，亦可采用高速离心代替过膜，取上清液上机，回收率更佳，推荐使用SHIMSEN低吸附PP材质样品瓶(1.5mL瓶盖垫组合，PN：380-00511 & 380-00503)；

3

亲和柱尽量不要重复使用 (每次使用后，柱容量都会降低，重复使用可能造成检测结果偏低)；

4

过柱时建议采用重力流出，保证样品与填料充分反应，回收率更有保障。

02

分析方法
(梯度优化，兼容大体积进样)

仪器：高效液相色谱仪配置二元梯度泵、自动进样器和紫外检测器

色谱柱：ShimNex WP C4-S(5 μm, 4.6×250 mm, PN: 380-01236-19)

(初次使用时，建议采用标准品溶液连续进样，至响应趋于稳定后，再进行测试)

柱温：25 ℃

检测波长：280 nm

流速：1.0 mL/min

进样量：10 μL

流动相

A：0.1%三氟乙酸水溶液

B：乙腈

标准品色谱图

梯度优化后，浓度: 200 μg/mL

*数据来源：“从此新生”挑战赛23号参赛者

样品重复进样谱图

乳粉样品，n=3

*数据来源：“从此新生”挑战赛23号参赛者

曲线线性

低吸附PP样品瓶，浓度范围0~200μg/mL，R2>0.999

样品重复进样谱图（峰型拖尾）

标准一致梯度，乳粉样品，n=3

参考文献

[1] 关于发布《食品安全国家标准食品添加剂使用标准》（GB 2760-2024）等47项食品安全国家标准和6项修改单的公告（2024年第1号），国家卫生健康委员会?国家市场监管总局

[2] GB 5009.299-2024 食品安全国家标准食品中乳铁蛋白的测定

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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.*', $join = Array)
[8]未定义数组索引: center
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: cid
[8]未定义数组索引: goods_list
[8]未定义数组下标: 0
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: center
[8]未定义数组索引: center
[2]Declaration of app\common\model\Tag::getAllList($filter = Array, $with = Array, $limit = 5) should be compatible with app\common\model\BaseModel::getAllList($filter = Array, $with = Array, $limit = 0, $sort = Array, $field = 'a.*', $join = Array)
[2]Declaration of app\common\model\Tag::remove($filter) should be compatible with app\common\model\BaseModel::remove($filter = Array)
[8]未定义数组索引: center
[8]未定义数组索引: wtt_list

[ DB ] CONNECT:[ UseTime:0.000326s ] mysql:host=127.0.0.1;port=3306;dbname=120med;charset=utf8
[ SQL ] SHOW COLUMNS FROM `tech_news_category` [ RunTime:0.000960s ]
[ SQL ] SELECT `id`,`name` FROM `tech_news_category` WHERE `is_show` = 1 [ RunTime:0.000350s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `parent_id` = 0 AND `is_show` = 1 ORDER BY `sort` ASC,`id` DESC [ RunTime:0.000311s ]
[ SQL ] SHOW COLUMNS FROM `company` [ RunTime:0.001137s ]
[ SQL ] SHOW COLUMNS FROM `tech_news` [ RunTime:0.000744s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `md5` = 'f9cf9b335c08e177' AND `review_status` = 1 LIMIT 1 [ RunTime:0.000255s ]
[ SQL ] SHOW COLUMNS FROM `user_info` [ RunTime:0.000824s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` = 203 [ RunTime:0.000683s ]
[ SQL ] SELECT * FROM `company` WHERE `id` = 321 [ RunTime:0.000228s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_text` [ RunTime:0.000725s ]
[ SQL ] SELECT * FROM `tech_news_text` WHERE `tech_news_id` = 3717 [ RunTime:0.014785s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_belong_category` [ RunTime:0.000944s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3717 [ RunTime:0.000918s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `id` IN (8) [ RunTime:0.000202s ]
[ SQL ] SHOW COLUMNS FROM `user_follow` [ RunTime:0.000829s ]
[ SQL ] SELECT `id` FROM `user_follow` WHERE `user_id` IS NULL AND `follow_user_id` = 203 LIMIT 1 [ RunTime:0.000194s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_comment` [ RunTime:0.000770s ]
[ SQL ] SELECT * FROM `tech_news_comment` WHERE `tech_news_id` = 3717 AND `parent_id` = 0 ORDER BY `id` DESC [ RunTime:0.000338s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `tech_news_comment` WHERE `tech_news_id` = 3717 LIMIT 1 [ RunTime:0.000143s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `is_show` = 1 AND `review_status` = 1 AND `id` IN (3717,1158,3854,3817,3789,3742,3692,3647,3456,3353) ORDER BY field(id,3717,1158,3854,3817,3789,3742,3692,3647,3456,3353) [ RunTime:0.000405s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (203,156,399,235,696,308,210,474,609,297) [ RunTime:0.000702s ]
[ SQL ] SHOW COLUMNS FROM `topic` [ RunTime:0.000842s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `topic` WHERE `review_status` = 1 ORDER BY `id` DESC LIMIT 4 [ RunTime:0.000155s ]
[ SQL ] SHOW COLUMNS FROM `topic_info_list` [ RunTime:0.000759s ]
[ SQL ] SELECT * FROM `topic_info_list` WHERE `topic_id` = 1 ORDER BY `id` DESC LIMIT 2 [ RunTime:0.000287s ]
[ SQL ] SHOW COLUMNS FROM `news` [ RunTime:0.000760s ]
[ SQL ] SELECT * FROM `news` WHERE `id` IN (864,849) [ RunTime:0.000203s ]
[ 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:0.000156s ]
[ SQL ] SHOW COLUMNS FROM `user` [ RunTime:0.000807s ]
[ 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:0.004615s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (592,413,444,224,13,239,598,697,394,285) [ RunTime:0.000743s ]
[ SQL ] SHOW COLUMNS FROM `seo` [ RunTime:0.000758s ]
[ SQL ] SELECT * FROM `seo` WHERE `column_type` = '16' AND `page_type` = 'tech_news' AND `info_id` = 3717 LIMIT 1 [ RunTime:0.000174s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3717 [ RunTime:0.000911s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1158 [ RunTime:0.001004s ]
[ SQL ] SHOW COLUMNS FROM `tag` [ RunTime:0.000826s ]
[ SQL ] SELECT `md5` FROM `tag` WHERE `is_open` = 1 AND `tag` = '标准' LIMIT 1 [ RunTime:0.000191s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3854 [ RunTime:0.000842s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3817 [ RunTime:0.000846s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3789 [ RunTime:0.000823s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3742 [ RunTime:0.000838s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3692 [ RunTime:0.000837s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3647 [ RunTime:0.000886s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3456 [ RunTime:0.000861s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3353 [ RunTime:0.000918s ]
[ SQL ] SELECT * FROM `user` WHERE `id` = 203 LIMIT 1 [ RunTime:0.000271s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 592 LIMIT 1 [ RunTime:0.000185s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 592 LIMIT 1 [ RunTime:0.000194s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 413 LIMIT 1 [ RunTime:0.000135s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 413 LIMIT 1 [ RunTime:0.000157s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 444 LIMIT 1 [ RunTime:0.000158s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 444 LIMIT 1 [ RunTime:0.000135s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 224 LIMIT 1 [ RunTime:0.000304s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 224 LIMIT 1 [ RunTime:0.000113s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 13 LIMIT 1 [ RunTime:0.000114s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 13 LIMIT 1 [ RunTime:0.000155s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 239 LIMIT 1 [ RunTime:0.000150s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 239 LIMIT 1 [ RunTime:0.000128s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 598 LIMIT 1 [ RunTime:0.000276s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 598 LIMIT 1 [ RunTime:0.000128s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 697 LIMIT 1 [ RunTime:0.000109s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 697 LIMIT 1 [ RunTime:0.000260s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 394 LIMIT 1 [ RunTime:0.000137s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 394 LIMIT 1 [ RunTime:0.000111s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 285 LIMIT 1 [ RunTime:0.000309s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 285 LIMIT 1 [ RunTime:0.000120s ]

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