高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物

目的 建立高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物的方法.方法 样品经甲醇超声提取,提取液离心、过微孔滤膜后上机分析.采用Waters Xbridge C18色谱柱(250 mm×4.6 mm,5 μm)分离,以20 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱,外标法定量测定.结果 在0.5~100.0 μg/mL的范围内2种新型卡巴地那非类似物线性关系良好(r2>0.999),定量限均为5 mg/kg.2种新型卡巴地那非类似物于1、2、10倍定量限3个水平下的平均回收率范围为87.32%~93.92%,相对标准偏差为1.19%~4.08%.采用该方法共检出8批次...

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Published in食品安全质量检测学报 Vol. 16; no. 3; pp. 235 - 240
Main Authors 吴婉琴, 江丰, 朱松松, 夏金涛, 范小龙, 张亚珍, 韩智, 张莉, 冯猛
Format Journal Article
LanguageChinese
Published 湖北省食品质量安全监督检验研究院,武汉 430075 2025
国家市场监督管理总局重点实验(动物源性食品中重点化学危害物检测技术),武汉 430075
湖北时珍实验室,武汉 430065%沃特世科技(上海)有限公司,上海 201206
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ISSN2095-0381
DOI10.19812/j.cnki.jfsq11-5956/ts.20240828002

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Abstract 目的 建立高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物的方法.方法 样品经甲醇超声提取,提取液离心、过微孔滤膜后上机分析.采用Waters Xbridge C18色谱柱(250 mm×4.6 mm,5 μm)分离,以20 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱,外标法定量测定.结果 在0.5~100.0 μg/mL的范围内2种新型卡巴地那非类似物线性关系良好(r2>0.999),定量限均为5 mg/kg.2种新型卡巴地那非类似物于1、2、10倍定量限3个水平下的平均回收率范围为87.32%~93.92%,相对标准偏差为1.19%~4.08%.采用该方法共检出8批次阳性样品,含量范围为218~2170mg/kg.结论 该方法操作简便,准确可靠,满足压片糖果和固体饮料中非法添加2种新型卡巴地那非类似物的含量测定,为打击食品中非法添加新型那非类物质提供可行的技术手段.
AbstractList 目的 建立高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物的方法.方法 样品经甲醇超声提取,提取液离心、过微孔滤膜后上机分析.采用Waters Xbridge C18色谱柱(250 mm×4.6 mm,5 μm)分离,以20 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱,外标法定量测定.结果 在0.5~100.0 μg/mL的范围内2种新型卡巴地那非类似物线性关系良好(r2>0.999),定量限均为5 mg/kg.2种新型卡巴地那非类似物于1、2、10倍定量限3个水平下的平均回收率范围为87.32%~93.92%,相对标准偏差为1.19%~4.08%.采用该方法共检出8批次阳性样品,含量范围为218~2170mg/kg.结论 该方法操作简便,准确可靠,满足压片糖果和固体饮料中非法添加2种新型卡巴地那非类似物的含量测定,为打击食品中非法添加新型那非类物质提供可行的技术手段.
Abstract_FL Objective To establish a method for determination of 2 kinds of new carbadenafil analogue in tablet candies and solid beverages by high performance liquid chromatography.Methods The sample was extracted by methanol ultrasound,the extract was centrifuged,filtered through a microporous membrane,and analyzed by the high performance liquid chromatography.The separation was performed on a Waters Xbridge C18 column(250 mmx4.6 mm,5 μm)with gradient elution by using 20 mmol/L ammonium acetate aqueous solution and methanol as the mobile phase,and quantified by external standard method.Results The 2 kinds of new carbadenafil analogue demonstrated good linearity in the range of 0.5-100.0 μg/mL,with the correlation coefficient values(r2)being higher than 0.999.The limits of quantification were found to be 5 mg/kg.The recoveries at 3 spiked levels of 1,2 and 10 times the limits of quantification in blank matrix were in the range of 87.32%-93.92%,with the relative standard deviations between 1.19%-4.08%.A total of 8 batches of positive samples were detected using this method,with a content range of 218-2170 mg/kg.Conclusion The method is convenient,accurate and efficient.It can meet the identification requirement of illegally added 2 kinds of new carbadenafil analogue in tablet candies and solid beverages,and provide effective technical support to combat the illegal addition of new carbadenafil analogue in food.
Author 朱松松
韩智
张莉
冯猛
吴婉琴
夏金涛
范小龙
江丰
张亚珍
AuthorAffiliation 湖北省食品质量安全监督检验研究院,武汉 430075;国家市场监督管理总局重点实验(动物源性食品中重点化学危害物检测技术),武汉 430075;湖北时珍实验室,武汉 430065%沃特世科技(上海)有限公司,上海 201206
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Author_FL WU Wan-Qin
JIANG Feng
ZHANG Li
FENG Meng
XIA Jin-Tao
ZHANG Ya-Zhen
HAN Zhi
ZHU Song-Song
FAN Xiao-Long
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DocumentTitle_FL Determination of 2 kinds of new carbadenafil analogue in tablet candies and solid beverages by high performance liquid chromatography
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Keywords 固体饮料
high performance liquid chromatography
压片糖果
tablet candies
illegal additions
solid beverages
高效液相色谱法
非法添加
carbadenafil analogue
卡巴地那非类似物
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PublicationTitle 食品安全质量检测学报
PublicationTitle_FL Journal of Food Safety & Quality
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Publisher 湖北省食品质量安全监督检验研究院,武汉 430075
国家市场监督管理总局重点实验(动物源性食品中重点化学危害物检测技术),武汉 430075
湖北时珍实验室,武汉 430065%沃特世科技(上海)有限公司,上海 201206
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Snippet 目的 建立高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物的方法.方法 样品经甲醇超声提取,提取液离心、过微孔滤膜后上机分析.采用Waters Xbridge C18色谱柱(250 mm×4.6 mm,5 μm)分离,以20 mmol/L乙酸铵水溶液和甲醇为流动相进行梯度洗脱,外标法定量测定.结果...
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Title 高效液相色谱法测定压片糖果和固体饮料中2种新型卡巴地那非类似物
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