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

中文关键词:  高效液相色谱法，卡巴地那非类似物，食品，非法添加

英文关键词:high performance liquid chromatography  carbadenafil analogue  tablet candies  solid beverages  illegal additions

中文摘要:

      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 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218~2170 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。

英文摘要:

      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 mm×4.6 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.