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| Qualitative and Quantitative Identification of a New Carbadenafil Analogue in Solid Beverages |
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| DOI： |
| KeyWord:coffee ?carbadenafil analogs ?illegal addition ?structure identification ?quantitative analysis |
| Author | Institution |
| XIA Jin-tao，WU Wan-qin，ZHU Song-song，JIANG Feng，FAN Zhi-yong，WANG Hui-xia，PENG Qing-zhi，YANG Zong |
1. Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test，Hubei Provincial Institute for Food Supervision and Test，Wuhan ，China;2. SCIEX，Shanghai ，China |
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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. |
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