Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages

XIA Jin-tao; WU Wan-qin; ZHU Song-song; JIANG Feng; FAN Zhi-yong; WANG Hui-xia; PENG Qing-zhi; YANG Zong

doi:10.19969/j.fxcsxb.21082001

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Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages

Scientific Papers | 更新时间：2022-06-22

- Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages
- Journal of Instrumental Analysis Vol. 41, Issue 5, Pages: 754-760(2022)
- 作者机构：
  
  1.湖北省食品质量安全监督检验研究院，湖北省食品质量安全检测工程技术研究中心，湖北武汉 430075
  2.上海爱博才思分析仪器贸易有限公司，上海 200335
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21082001
  CLC：
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夏金涛,吴婉琴,朱松松等.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(05):754-760.

XIA Jin-tao,WU Wan-qin,ZHU Song-song,et al.Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages[J].Journal of Instrumental Analysis,2022,41(05):754-760.
夏金涛,吴婉琴,朱松松等.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(05):754-760. DOI： 10.19969/j.fxcsxb.21082001.

XIA Jin-tao,WU Wan-qin,ZHU Song-song,et al.Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages[J].Journal of Instrumental Analysis,2022,41(05):754-760. DOI： 10.19969/j.fxcsxb.21082001.

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（,r,2,）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。

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（,r,2,） 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.

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

Keywords

coffeecarbadenafil analogsillegal additionstructure identificationquantitative analysis

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Technology Center of Changsha Customs

China Certification＆Inspection Group Hunan Co.，Ltd.

Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine，Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals，Institute of Analysis，Guangdong Academy of Sciences（China National Analytical Center，），Guangzhou

Institute of Analysis，Guangdong Academy of Sciences（China National Analytical Center，Guangzhou），Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology，Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine

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