| 固体饮料中一种新型卡巴地那非类似物的定性鉴别和定量分析 |
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| 基金项目:湖北省重点研发计划项目（2020BCA091） |
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| 中文摘要:采用超高效液相色谱 - 四极杆 - 飞行时间高分辨质谱（UPLC - Q - TOF MS）、超高效液相色谱 - 线性离子阱/静电场轨道阱高分辨质谱（UPLC - LTQ/Orbitrap MS）筛查出固体饮料中一种新型的、结构未知的非法添加卡巴地那非类似物。经核磁共振（Bruker）一维、二维谱和文献分析，确定该物质为N-苯基丙氧苯基卡巴地那非。通过高效液相色谱 - 串联质谱（HPLC - MS/MS）外标法定量分析表明，N-苯基丙氧苯基卡巴地那非在2～50 ng/mL质量浓度范围内线性关系良好，相关系数（r2）为0.999 1，方法检出限为0.05 mg/kg，定量下限为0.1 mg/kg，在低、中、高3个加标水平下的平均回收率为89.2%～93.1%，相对标准偏差（RSD）为1.8%～3.1%。采用该方法测定10批次固体饮料，发现5批次阳性样品，N-苯基丙氧苯基卡巴地那非的检出含量为214～880 mg/kg。该方法的准确度高、灵敏度好，可作为筛查非法添加卡巴地那非类似物的有效方法。 |
| 中文关键词:咖啡 ?卡巴地那非类似物 ?非法添加 ?结构鉴定 ?定量分析 |
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| Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages |
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| Abstract:A high performance liquid chromatography - tandem mass spectrometry（HPLC - MS/MS）was developed for the qualitative and quantitative identification of a novel，illegally added and unknown carbadenafil analogue，N-phenylpropoxyphenyl carbadenafil in solid beverages.The sample was firstly identified by using ultra-performance liquid chromatography－quadrupole time-of-flight mass spectrometry（UPLC - Q - TOF MS） and ultra-performance liquid chromatography - linear ion trap/orbitrap high resolution mass spectrometry（UPLC－LTQ/Orbitrap MS）.Then the structure of this compound was finally determined as N-phenylpropoxyphenyl carbadenafil by one-dimensional and two-dimensional nuclear magnetic resonance（NMR） spectra and textual comparison.Quantitative analysis was carried out by the external standard method. Results showed that there was a good linear relationship for the analyte in the range of 2 - 50 ng/mL，with correlation coefficient（r2） of 0.999 1.The limit of detection（LOD） and quantification（LOQ） were 0.05 mg/kg and 0.1 mg/kg，respectively. Recoveries at low，medium and high spiked levels ranged from 89.2% to 93.1%， with relative standard deviations（RSD）of 1.8% - 3.1%. Determination on 10 batches of coffee solid beverages revealed that 5 batches of samples were found to be positive，and the contents of N-phenylpropoxyphenyl carbadenafil were between 214 mg/kg and 880 mg/kg. With high accuracy and high efficiency，this method is effective for the screening of illegally added carbadenafil analogs beyond the detection range of current standard. |
| Key Words:coffee ?carbadenafil analogs ?illegal addition ?structure identification ?quantitative analysis |
| 引用本文：夏金涛，吴婉琴，朱松松，江丰，范志勇，王会霞，彭青枝，杨总.固体饮料中一种新型卡巴地那非类似物的定性鉴别和定量分析[J].分析测试学报,2022,41(5):754-760. |
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