Screening and Quantitative Determination of a New Vardenafil Analogue in Foods

LIU Ya-ting; GUO Yu-xin; LIU Zhen-qiang; LIU Jian-ping; WANG Huan; LIU Yang; DAI Jie-yun; WANG Mei-ling

doi:10.19969/j.fxcsxb.23042404

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Screening and Quantitative Determination of a New Vardenafil Analogue in Foods

Experimental Techniques and Methods | 更新时间：2023-11-10

- Screening and Quantitative Determination of a New Vardenafil Analogue in Foods
- Journal of Instrumental Analysis Vol. 42, Issue 11, Pages: 1488-1494(2023)
- 作者机构：
  
  1.中国检验认证集团湖南有限公司，湖南长沙 410021
  2.长沙海关技术中心，湖南长沙 410004
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23042404
  CLC：
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刘雅婷,郭予昕,刘振强等.食品中一种新型伐地那非结构类似物的筛查与定量测定[J].分析测试学报,2023,42(11):1488-1494.

LIU Ya-ting,GUO Yu-xin,LIU Zhen-qiang,et al.Screening and Quantitative Determination of a New Vardenafil Analogue in Foods[J].Journal of Instrumental Analysis,2023,42(11):1488-1494.
刘雅婷,郭予昕,刘振强等.食品中一种新型伐地那非结构类似物的筛查与定量测定[J].分析测试学报,2023,42(11):1488-1494. DOI： 10.19969/j.fxcsxb.23042404.

LIU Ya-ting,GUO Yu-xin,LIU Zhen-qiang,et al.Screening and Quantitative Determination of a New Vardenafil Analogue in Foods[J].Journal of Instrumental Analysis,2023,42(11):1488-1494. DOI： 10.19969/j.fxcsxb.23042404.

摘要

采用液相色谱-四极杆飞行时间高分辨质谱在压片糖果中发现一种与伐地那非结构类似的化合物。依据高分辨质谱碎片离子推测该伐地那非结构类似物的分子结构及裂解规律，结合红外光谱和核磁共振谱分析鉴定，确定该化合物为丙氧基伐地那非。高效液相色谱-串联质谱外标法定量分析表明，丙氧基伐地那非在1.0~100 ng/mL质量浓度范围内线性关系良好，相关系数（,r,2,）为0.999 2，方法检出限为0.02 mg/kg，定量下限为0.05 mg/kg，在压片糖果、保健酒及蜂蜜酱基质中3个加标水平下的平均回收率为76.5%~104%，相对标准偏差（RSD）为1.6%~5.1%。采用该方法测定实际样品，发现5批次糖果（含压片糖果）和3批次保健酒为阳性样品。该方法具有快速、准确、灵敏度高等优点，可作为非法添加伐地那非结构类似物的有效筛查方法。

Abstract

A novel vardenafil analogue was detected in a pressed candy by liquid chromatography-quadrupole time-of-flight mass spectrometry. The molecular structure and fragmentation law of the compound were inferred from the fragment ions identified by high-resolution mass spectrometry. Its structure was further confirmed by IR spectrum and NMR spectrum. The compound was finally identified and confirmed as O-propylvardenafil. Quantitative analysis was carried out by high performance liquid chromatography-tandem mass spectrometry with the external standard method. Results showed that there was a good linear relationship for the analyte in the range of 1.0-100 ng/mL，with correlation coefficient（,r,2,）of 0.999 2.The limit of detection and limit of quantitation were 0.02 mg/kg and 0.05 mg/kg，respectively. Recoveries at low，medium and high spiked levels were ranged from 76.5%-104%，with relative standard deviations（RSDs） of 1.6%-5.1%. The method was applied to the detection of real samples. The results showed that 5 batches of candy including pressed candy and 3 batches of health wine were positive samples. This method is rapid，accurate and high sensitive，and can be used as an effective method for screening and identification of vardenafil analogue.

关键词

伐地那非结构类似物非法添加液相色谱-四极杆飞行时间高分辨质谱食品

Keywords

vardenafil analogueillegal additionliquid chromatography-quadrupole time-of-flight mass spectrometryfoods

references

Wang Z L，Liang B W，Dong P Z，Liu W B，Wang K，Xiang X H. China Food Addit. 王子龙，梁卜文，董培智，刘文博，王珂，项新华. 中国食品添加剂），2021，（1）：64-71.

Dong P Z，Shen G H，Wang Z L，Guo J W，Xing J S. Chin. J. Mod. Appl. Pharm.（董培智，申国华，王子龙，郭景文，行江水. 中国现代应用药学），2018，40（12）：2798-2802.

Xia J，Yao H，Du L P，Chen H J，Xi S D. Chin. J. Mod. Appl. Pharm.（夏佳，姚慧，杜吕佩，陈红娟，席时东. 中国现代应用药学），2017，34（8）：1167-1170.

Wang K，Dong P Z，Shen G H，Zhang L，Liang B W，Guo J W. Chin. Pharm. Aff. （王珂，董培智，申国华，张禄，梁卜文，郭景文. 中国药事），2019，33（4）：429-434.

Xia J T，Wu W Q，Zhu S S，Jiang F，Fan Z Y，Wang H X，Peng Q Z，Yang Z. J. Instrum. Anal.（夏金涛，吴婉琴，朱松松，江丰，范志勇，王会霞，彭青枝，杨总. 分析测试学报），2022，41（5）：754-760.

Zeng L H，Li S Y，Li W Q，Li Y J，Huang M. Guangdong Chem. Ind.（曾令浩，李思颖，李文倩，李俞洁，黄密. 广东化工），2022，24（49）：275-278.

Feng T T，Sun J，Zhang J X，Yu H，Feng R，Zhang S，Mao X H，Hu Q，Ji S. Acta Pharm. Sin.（冯亭亭，孙健，张静娴，于泓，冯睿，张甦，毛秀红，胡青，季申. 药学学报），2020，55（8）：1877-1881.

Chen Y，Yan L J，Xu D M，Li C Y，Sun T. J. Instrum. Anal.（陈燕，严丽娟，徐敦明，黎翠玉，孙婷. 分析测试学报），2023，42（5）：519-530.

Feng R，Yu H，Sun J，Hu Q，Zhang S，Mao X H，Ji S. J. Food Saf. Qual. （冯睿，于泓，孙健，胡青，张甦，毛秀红，季申. 食品安全质量检测学报），2016，7（7）：2710-2714.

Sun J，Yu H，Hu Q，Feng R，Zhang S，Ji S. Acta Pharm. Sin.（孙健，于泓，胡青，冯睿，张甦，季申. 药学学报），2014，49（4）：513-516.

Huang Z H，Cai D D，Zhuo K H. Chin. J. Mod. Appl. Pharm.（黄朝辉，蔡丹丹，卓开华. 中国现代应用药学），2018，35（7）：991-994.

Liu Y W，Zou Y H，Yin H M. Chin. Pharm. J. （刘宇文，邹耀华，殷红妹. 中国药学杂志），2016，51（23）：2059-2062.

Vehuis B J，Kaste D. J. Pharm. Biomed. Anal.，2012，69：196-208.

Kern S E，Nickum E A，Flurer R A，Toomey V M，Litzau J J. J. Pharm. Biomed. Anal.，2015，103：99-103.

BJS 201601. Determination of Phosphodiesterase 5（PDE5） Inhibitors in Foods. China Food and Drug Administration，Additional Testing Methods（食品中那非类物质的测定. 国家食品药品监督管理总局食品补充检验方法）.

BJS 201704. Determination of Nortadalafil and Thiosildenafil in Foods by High Performance Liquid Chromatography Tandem Mass Spectrometry. China Food and Drug Administration，Additional Testing Methods（食品中去甲基他达拉非和硫代西地那非的测定高效液相色谱-串联质谱法. 国家食品药品监督管理总局食品补充检验方法）. （下转第1502页）

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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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Hubei Provincial Engineering and Technology Research Center for Food Quality and Safety Test，Hubei Provincial Institute for Food Supervision and Test

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