Nguyễn Văn Sỹ, Lê Hồng Dũng

Nội dung chính của bài viết

Tóm tắt

Aims: A rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was validated for determination of prohibited cyproheptadine hydrochloride (CP) in dietary supplements.

Methods: CP was extracted by sonication in methanol for 30 min. The chromatography separation of CP took place on C18 column (100 mm x 2.1 mm, 1.8 µm) with gradient mobile phase of both of acetonitrile and water containing 0.1% formic acid. Multiple reaction monitoring (MRM) in the positive mode was used to quantify and confirm CP at m/z 288.2/191.1  and 288.1/96.0, respectively.

Results: The method was validated according to the AOAC requirements. The linearity ranges were found from 0.1 to 50 ng. mL-1 of CP (R2 = 1). The limit of detection and limit of quantification were 1.5 ng/g or ng/mL and 5 ng/g or ng/mL, respectively. The accuracy was within the range from 92 to 99%, with the relative standard deviation (RSD%) of 2.0-5.9%.

Conclusion: The validated parameters have met the requirement of Association of Official Agricultural Chemists (AOAC). This reliable method would be useful for the monitoring of cyproheptadine in dietary supplements.

Chi tiết bài viết

Tài liệu tham khảo

1. Hassan Y and Al-Badr A (1981). Cyproheptadine. Analytical Profiles of Drug Substances
2. Yuan CM, Spandorfer PR, Miller SL, Henretig FM. Shaw LM (2003). Evaluation of tricyclic antidepressant false positivity an a pediatric case of cyproheptadine (periactin) overdose. Ther Drug Monit 25(3): 299-304
3. Sushil D. Patil, Tejashri Dugaje, Sanjay J. Kshirsagar (2019). Development and Validation of UV Spectrophotometric Method for Estimation of Cyproheptadine hydrochloride. Asian Journal of Research in Chemistry: 12(2).
4. Alaa el-Gindy, Fawzy el-Yazby, Ahmed Mostafa, Moustafa M. Maher (2004). HPLC and chemometric method for the simultaneous determination of cyproheptadine hydrochloride, multivitamins, and sorbic acid. J Pharm Biomed Anal 35(4):703-713
5. Maha M Abdelrahman, Eglal A Abdelaleem, Nouruddin W Ali, Raghda A Emam (2021). Development and Validation of Stability Indicating High-Performance Liquid Chromatographic Method for Determination of Cyproheptadine Hydrochloride, its Impurity and Degradation Product. Journal of Chromatographic Science 59(2):128-133
6. Feas X, Ye L, Hosseini SV, Fente CA, Cepeda A (2009). Development and validation of LC-MS/MS method for the determination of cyproheptadine in several pharmaceutical syrup formulations. J Pharm Biomed Anal 50(5):1044-1049.
7. The Ministry of Dietary, Vietnam (2021). Circula 10/2011/TT-BYT .
8. The European Commission (2021). Commission Implementing Regulation (EU) 2021/808. Official Journal of the European Union 180: 84-109
9. AOAC Official Method Analysis (2016). Appendix F. Guidelines for Standard Method Performance Requirements. Appendix F, p.2.