特色方案｜余干子中没食子酸和鞣花酸的测定-医疗器械网

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特色方案｜余干子中没食子酸和鞣花酸的测定

来源：岛津（上海）实验器材有限公司分类：应用方案 2023-11-23 17:33:49 9阅读次数

余干子中没食子酸和

鞣花酸的测定

ShimNex CS C18 HPLC

本文建立了余干子中没食子酸和鞣花酸的 HPLC 测定方法。参照新公示稿中色谱条件，采用色谱柱ShimNex CS C18 分析余干子中没食子酸和鞣花酸，结果显示，没食子酸和鞣花酸峰型对称，理论塔板数按没食子酸峰计算大于 4000，没食子酸和鞣花酸均与相邻杂质峰基线分离，满足新公示稿要求。此方法可为余干子中没食子酸和鞣花酸的检测提供参考。

“

PART ONE

实验部分

1.1 实验仪器及耗材

Shimadzu LC-20AD 高效液相色谱仪；

色谱柱：ShimNex CS C18（5 μm，4.6×250mm；P/N：380-01230-01）；

纯水机：PR-FP-0120α-MT1（+60L水箱+取水器）

SHIMSEN Arc Disc HPTFE 针式过滤器（P/N：380-00341-05）；

LC/MS认证样品瓶 LabTotal Vial（ P/N：227-34001-01）；

SHIMSEN Pipet 移液枪：SHIMSEN Pipet PMII-10（ P/N：380-00751-02）；

SHIMSEN Pipet PMII-100（ P/N：380-00751-04）；

SHIMSEN Pipet PMII-1000（ P/N：380-00751-06）。

1.2 对照品溶液的制备

取没食子酸对照品、鞣花酸对照品适量，精密称定，加甲醇制成每 1mL 各含 20μg 的混合溶液，摇匀，即得。

1.3 供试品溶液的制备

取本品粉末（过三号筛）约 0.1g，精密称定，置具塞锥形瓶中，精密加入甲醇 50 mL，密塞，称定重量，超声处理（功率 200 W，频率 40 kHz）30 分钟，放冷，再称定重量，用甲醇补足减失的重量，摇匀，滤过，取续滤液，即得。

1.4 分析条件

色谱柱：ShimNex CS C18（5μm，4.6×250mm；P/N：380-01230-01）

流速：1.0 mL/min

进样量：5 μL

柱温：30 ℃

检测波长：270 nm

流动相：A：0.2% 磷酸水溶液

B：甲醇

“

PART TWO

实验部分

按照上述色谱条件（1.4）进行采集，对照品溶液和供试品溶液色谱图如下：

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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
[8]未定义数组索引: center
[8]未定义数组索引: wtt_list

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[ SQL ] SHOW COLUMNS FROM `tech_news_category` [ RunTime:0.000978s ]
[ SQL ] SELECT `id`,`name` FROM `tech_news_category` WHERE `is_show` = 1 [ RunTime:0.000434s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `parent_id` = 0 AND `is_show` = 1 ORDER BY `sort` ASC,`id` DESC [ RunTime:0.000171s ]
[ SQL ] SHOW COLUMNS FROM `company` [ RunTime:0.000830s ]
[ SQL ] SHOW COLUMNS FROM `tech_news` [ RunTime:0.000867s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `md5` = 'e1ff91edf9e54d73' AND `review_status` = 1 LIMIT 1 [ RunTime:0.000250s ]
[ SQL ] SHOW COLUMNS FROM `user_info` [ RunTime:0.000881s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` = 203 [ RunTime:0.000736s ]
[ SQL ] SELECT * FROM `company` WHERE `id` = 321 [ RunTime:0.000376s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_text` [ RunTime:0.000798s ]
[ SQL ] SELECT * FROM `tech_news_text` WHERE `tech_news_id` = 1654 [ RunTime:0.015570s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_belong_category` [ RunTime:0.000980s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1654 [ RunTime:0.000974s ]
[ SQL ] SELECT * FROM `tech_news_category` WHERE `id` IN (5) [ RunTime:0.000294s ]
[ SQL ] SHOW COLUMNS FROM `user_follow` [ RunTime:0.000803s ]
[ SQL ] SELECT `id` FROM `user_follow` WHERE `user_id` IS NULL AND `follow_user_id` = 203 LIMIT 1 [ RunTime:0.000185s ]
[ SQL ] SHOW COLUMNS FROM `tech_news_comment` [ RunTime:0.000762s ]
[ SQL ] SELECT * FROM `tech_news_comment` WHERE `tech_news_id` = 1654 AND `parent_id` = 0 ORDER BY `id` DESC [ RunTime:0.000201s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `tech_news_comment` WHERE `tech_news_id` = 1654 LIMIT 1 [ RunTime:0.000296s ]
[ SQL ] SELECT * FROM `tech_news` WHERE `is_show` = 1 AND `review_status` = 1 AND `id` IN (1654,1653,3905,3865,3859,3834,3832,3825,3795,3783) ORDER BY field(id,1654,1653,3905,3865,3859,3834,3832,3825,3795,3783) [ RunTime:0.000459s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (203,345,722,598,530,262,307,353) [ RunTime:0.000886s ]
[ SQL ] SHOW COLUMNS FROM `topic` [ RunTime:0.000935s ]
[ SQL ] SELECT `id`,`md5`,`title`,`created_time` FROM `topic` WHERE `review_status` = 1 ORDER BY `id` DESC LIMIT 4 [ RunTime:0.000158s ]
[ SQL ] SHOW COLUMNS FROM `topic_info_list` [ RunTime:0.000874s ]
[ SQL ] SELECT * FROM `topic_info_list` WHERE `topic_id` = 1 ORDER BY `id` DESC LIMIT 2 [ RunTime:0.000171s ]
[ SQL ] SHOW COLUMNS FROM `news` [ RunTime:0.000889s ]
[ SQL ] SELECT * FROM `news` WHERE `id` IN (864,849) [ RunTime:0.000256s ]
[ 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:0.000329s ]
[ SQL ] SHOW COLUMNS FROM `user` [ RunTime:0.000775s ]
[ 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:0.005137s ]
[ SQL ] SELECT * FROM `user_info` WHERE `user_id` IN (592,413,444,224,13,239,598,697,394,285) [ RunTime:0.000732s ]
[ SQL ] SHOW COLUMNS FROM `seo` [ RunTime:0.000919s ]
[ SQL ] SELECT * FROM `seo` WHERE `column_type` = '16' AND `page_type` = 'tech_news' AND `info_id` = 1654 LIMIT 1 [ RunTime:0.000223s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1654 [ RunTime:0.000950s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 1653 [ RunTime:0.000966s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3905 [ RunTime:0.000919s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3865 [ RunTime:0.000878s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3859 [ RunTime:0.000870s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3834 [ RunTime:0.000890s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3832 [ RunTime:0.000925s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3825 [ RunTime:0.000893s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3795 [ RunTime:0.001054s ]
[ SQL ] SELECT * FROM `tech_news_belong_category` WHERE `tech_news_id` = 3783 [ RunTime:0.000963s ]
[ SQL ] SELECT * FROM `user` WHERE `id` = 203 LIMIT 1 [ RunTime:0.000261s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 592 LIMIT 1 [ RunTime:0.000227s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 592 LIMIT 1 [ RunTime:0.000164s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 413 LIMIT 1 [ RunTime:0.000160s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 413 LIMIT 1 [ RunTime:0.000146s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 444 LIMIT 1 [ RunTime:0.000183s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 444 LIMIT 1 [ RunTime:0.000244s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 224 LIMIT 1 [ RunTime:0.000177s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 224 LIMIT 1 [ RunTime:0.000124s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 13 LIMIT 1 [ RunTime:0.000150s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 13 LIMIT 1 [ RunTime:0.000167s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 239 LIMIT 1 [ RunTime:0.000133s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 239 LIMIT 1 [ RunTime:0.000114s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 598 LIMIT 1 [ RunTime:0.000115s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 598 LIMIT 1 [ RunTime:0.000117s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 697 LIMIT 1 [ RunTime:0.000119s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 697 LIMIT 1 [ RunTime:0.000118s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 394 LIMIT 1 [ RunTime:0.000109s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 394 LIMIT 1 [ RunTime:0.000108s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `follow_user_id` = 285 LIMIT 1 [ RunTime:0.000106s ]
[ SQL ] SELECT COUNT(*) AS tp_count FROM `user_follow` WHERE `user_id` = 285 LIMIT 1 [ RunTime:0.000109s ]

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