本文選題：消炎鎮(zhèn)痛藥 + 吡羅昔康片�。� 參考：《藥物分析雜志》2017年02期

【摘要】：目的:建立近紅外(NIR)模型識別吡羅昔康原料藥及片劑中原料藥的晶型,結(jié)合PⅡ晶型原料藥中1,2-二氯乙烷殘留量超標,建立GC-MS法快速分析PⅡ晶型原料藥生產(chǎn)的吡羅昔康片中1,2-二氯乙烷殘留。方法:利用近紅外光譜儀在12 000~4 000 cm~(-1)范圍內(nèi)采集吡羅昔康原料藥及片劑的近紅外光譜。分別針對吡羅昔康原料藥建立NIR聚類分析模型,對片劑進行二階導(dǎo)數(shù)化預(yù)處理,平滑點數(shù)21個,r閾值設(shè)置為97%,建立相關(guān)系數(shù)模型識別晶型差異;通過粉末X射線衍射法(PXRD法)驗證原料藥晶型識別結(jié)果。建立GC-MS方法測定吡羅昔康原料藥中1,2-二氯乙烷殘留;針對NIR相關(guān)系數(shù)模型篩選出吡羅昔康片PⅡ晶型的樣品,測定其1,2-二氯乙烷殘留。結(jié)果:PXRD和NIR聚類分析結(jié)果一致,吡羅昔康原料藥為PⅠ、PⅡ2種晶型;NIR模型判斷吡羅昔康片中14批樣品為PⅡ晶型,模型r閾值≥97%,剩余124批樣品的r閾值97%,為PⅠ晶型。GC-MS方法r為0.999 7,原料藥和片劑的回收率分別為91.5%和90.9%,檢出限為0.000 088%。GC-MS結(jié)果中,PⅡ類原料藥二氯乙烷含量為0.036 6%,超出標準限度,PⅠ類未檢出;NIR模型篩選出的PⅡ類吡羅昔康片中二氯乙烷含量均超出限度,PⅠ類片未檢出。結(jié)論:本方法通過對原料藥晶型的識別進而分析PⅡ晶型吡羅昔康片中1,2-二氯乙烷殘留,方法簡便快速,結(jié)果準確可靠。
[Abstract]:Objective: to establish a near infrared (NIR) model to identify the crystal form of Piroxicam and its tablets, and to combine with the PII crystal drug, the residual amount of 1h2- dichloroethane exceeded the standard. A GC-MS method was established for the rapid determination of 1H 2 dichloroethane residues in Piroxicam tablets. Methods: the near infrared spectra of Piroxicam raw materials and tablets were collected by near infrared spectrometer in the range of 12 000 ~ 4 000 cm ~ (-1). The NIR cluster analysis model was established for Piroxicam, and the second derivative pretreatment was carried out on the tablets. The threshold value of smooth number 21 r was set to 97, and the correlation coefficient model was established to identify the crystal type difference. The results of crystal pattern identification were verified by powder X ray diffraction (PXRD). A GC-MS method was established for the determination of 1h2- dichloroethane residues in Piroxicam crude drug, and the crystal form of Piroxicam tablets P 鈪，

本文編號：1900885