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  

Determination of 2 kinds of new carbadenafil analogue in tablet candies and solid beverages by high performance liquid chromatography

作　　者：吴婉琴 江丰 朱松松 夏金涛 范小龙 张亚珍 韩智 张莉 冯猛 WU Wan-Qin;JIANG Feng;ZHU Song-Song;XIA Jin-Tao;FAN Xiao-Long;ZHANG Ya-Zhen;HAN Zhi;ZHANG Li;FENG Meng(Hubei Provincial Institute for Food Supervision and Test,Wuhan 430075,China;Key Laboratory of Detection Technology of Focus Chemical Hazards in Animal-derived Food,State Administration for Market Regulation,Wuhan 430075,China;Hubei Shizhen Laboratory,Wuhan 430065,China;Waters Corporation,Shanghai 201206,China)

机构地区：[1]湖北省食品质量安全监督检验研究院,武汉430075 [2]国家市场监督管理总局重点实验室(动物源性食品中重点化学危害物检测技术),武汉430075 [3]湖北时珍实验室,武汉430065 [4]沃特世科技(上海)有限公司,上海201206

出　　处：《食品安全质量检测学报》2025年第3期235-240,共6页Journal of Food Safety and Quality

基　　金：国家市场监督管理总局科技计划项目(2024MK085);国家市场监督管理总局科技创新人才计划(青年拔尖人才)项目(QNBJ202330);国家重点研发计划项目(2023YFF1104700);国家市场监督管理总局科技计划项目(2022MK085)。

摘　　要：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 C_(18)色谱柱(250 mm×4.6 mm,5μm)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0.5~100.0μg/mL的范围内2种新型卡巴地那非类似物线性关系良好(r^(2)>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218~2170 mg/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。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 C_(18) column(250 mm×4.6 mm,5μm)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 0.5-100.0μg/mL,with the correlation coefficient values(r^(2))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.

关 键 词：高效液相色谱法 卡巴地那非类似物 压片糖果 固体饮料 非法添加 

分 类 号：O657.72[理学—分析化学] TS246.5[理学—化学] TS278[轻工技术与工程—制糖工程]