建立应急检验模型快速筛查及确证片剂中添加的枸橼酸西地那非

Establishment of Emergency Inspection Model for Rapid Screening and Identification of Sildenafil Citrate in Tablets

目的：建立近红外光谱联用超高效液相色谱四级杆飞行时间质谱应急检验模型，快速筛查及确证片剂中添加枸橼酸西地那非，为药品检测车载系统的应用提供参考。方法：采用近红外扫描，处理方法为二阶导数法，平滑点为13个，特征谱段为6200～5300cm^-1，相关系数阈值设为70％。将超过阈值的样品通过UPLC—DAD—ESI—Q—TOFMS分析，利用液相色谱保留时间、DAD紫外光谱图、一级质谱、二级质谱碎片4方面信息，对片剂中添加的枸橼酸西地那非进行快速定性鉴别。结果：经过近红外光谱应急检验模型初筛为阳性的样品采用UPLC-Q—ToFMS在3min左右时间内被快速确证含有西地那非。结论：建立的应急检验模型和超高效液相色谱四级杆飞行时间质谱法具有方法简单、易操作等特点，适用于大批量的筛查，并在几分钟内完成快速确证。

Objective： To establish an emergency inspection model by UPLC-DAD-ESI-Q-TOF MS for rapid screening and identification of sildenafil citrate in tablets so as to provide a reference for the application of drug testing vehicle system. Methods： The emergency inspection model was established with near infrared scan, all the spectra were preprocessed by second derivative with 13 smoothing points, the spectral range of 6200 - 5300 cm-1 was selected as the characteristic spectral band, and 70% was set as the threshold for related coefficients. Samples out of the threshold were analyzed by UPLC-DAD-ESI-Q-TOF MS. Sildenafil citrate in tablets was rapidly identified according to the information of four aspects including HPLC retention time, DAD ultraviolet spectra, the first order mass spectrum and fragment information of the second order mass spectrum. Results： For samples detected as positive through the near infrared emergency inspection model, the content of sildenafil citrate was quickly confirmed by UPLC-DAD-ESI-Q-TOF MS in approximately 3 min. Conclusion： The established emergency inspection model and UPLC-Q-TOF MS are simple and easy to operate, which could be applied for rapid screening of large quantities of samples and could rapidly confirm large quantities of samples in a few minutes.