NIDRS法结合GC-MS法分析吡罗昔康原料晶型及PⅡ晶型吡罗昔康片中1,2-二氯乙烷残留

发布时间：2018-05-17 09:43

  本文选题：消炎镇痛药 + 吡罗昔康片　； 参考：《药物分析杂志》2017年02期

【摘要】：目的:建立近红外(NIR)模型识别吡罗昔康原料药及片剂中原料药的晶型,结合PⅡ晶型原料药中1,2-二氯乙烷残留量超标,建立GC-MS法快速分析PⅡ晶型原料药生产的吡罗昔康片中1,2-二氯乙烷残留。方法:利用近红外光谱仪在12 000~4 000 cm~(-1)范围内采集吡罗昔康原料药及片剂的近红外光谱。分别针对吡罗昔康原料药建立NIR聚类分析模型,对片剂进行二阶导数化预处理,平滑点数21个,r阈值设置为97%,建立相关系数模型识别晶型差异;通过粉末X射线衍射法(PXRD法)验证原料药晶型识别结果。建立GC-MS方法测定吡罗昔康原料药中1,2-二氯乙烷残留;针对NIR相关系数模型筛选出吡罗昔康片PⅡ晶型的样品,测定其1,2-二氯乙烷残留。结果:PXRD和NIR聚类分析结果一致,吡罗昔康原料药为PⅠ、PⅡ2种晶型;NIR模型判断吡罗昔康片中14批样品为PⅡ晶型,模型r阈值≥97%,剩余124批样品的r阈值97%,为PⅠ晶型。GC-MS方法r为0.999 7,原料药和片剂的回收率分别为91.5%和90.9%,检出限为0.000 088%。GC-MS结果中,PⅡ类原料药二氯乙烷含量为0.036 6%,超出标准限度,PⅠ类未检出;NIR模型筛选出的PⅡ类吡罗昔康片中二氯乙烷含量均超出限度,PⅠ类片未检出。结论:本方法通过对原料药晶型的识别进而分析PⅡ晶型吡罗昔康片中1,2-二氯乙烷残留,方法简便快速,结果准确可靠。
[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，

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