救必应胃痛片质量标准的提升研究

Study on improving the quality standard of Jiubiying Weitong tablets

目的:完善和提高救必应胃痛片的质量标准,为有效控制该制剂内在质量提供实验依据。方法(:1)增加显微鉴别项,对处方中以细粉入药的木香、救必应、肉桂、陈皮和高良姜5种植物药材进行显微鉴别。(2)简化原标准中橙皮苷、桂皮醛和木香的薄层色谱鉴别法,增加木香烃内酯和去氢木香烃内酯的薄层色谱鉴别法。(3)简化及改进原标准中检测橙皮苷含量的高效液相色谱法,增加木香烃内酯、去氢木香烃内酯、桂皮醛3个含量控制指标成分,建立同时测定橙皮苷、木香烃内酯、去氢木香烃内酯和桂皮醛含量的方法。结果(:1)显微鉴别中,救必应胃痛片粉末具有与木香、救必应、肉桂、陈皮和高良姜等对照药材相应的显微特征。(2)薄层色谱鉴别中,橙皮苷、桂皮醛、木香烃内酯和去氢木香烃内酯的图谱清晰,与杂质斑点分离较好,阴性对照无干扰。(3)含量测定中,木香烃内酯、去氢木香烃内酯、橙皮苷、桂皮醛质量浓度分别在0.894 4~44.72μg·-1(r=0.999 3)、0.857 6~42.88μg·m L-1(r=0.999 3)、1.901~142.6μg·m L-1m L(r=0.999 2)、1.578~78.92μg·m L-1(r=0.999 0)范围内线性关系良好,平均回收率(n=6)分别为100.8%(RSD=2.1%)、101.2%(RSD=2.2%)、101.3%(RSD=2.7%)、96.2%(RSD=2.8%)。测定救必应胃痛片样品13批,其含量分别为:木香烃内酯0.011 6~0.200 8 mg·片-1;去氢木香烃内酯0.084 9~0.221 9 mg·片-1;橙皮苷0.711 7~1.232 0 mg·片-1;桂皮醛0.029 5~1.007 5 mg·片-1。结论:本文所建立和完善的显微鉴别法、薄层色谱法、4种含量控制指标成分的测定方法,方法简便,重现性好,专属性强,可用于救必应胃痛片的质量控制。

Objective：To perfect and improve the quality standard of the Jiubiying Weitong tablets and provide the experimental basis for the effective control of the inherent quality of the preparation.Methods（：1）For powder medicine Aucklandiae Radix,Ilicis Rotundae Cortex,Cinnamon Cortex,Citri Reticulatae Pericarpium and Alpinia officinarum Rhizoma in Jiubiying Weitong tablets,the microscopic identification was adopted.（2）To simplify the TLC methods of hesperidin、cinnamaldehyde and Aucklandiae Radix,TLC identifications of costunolide and dehydrocostuslactone were added.（3）To simplify and improve the HPLC methods of hesperidin in the original standard,the amount of costunolide、dehydrocostuslactone and cinnamaldehyde were added.An HPLC method for simultaneous determination of costunolide,dehydrocostuslactone,hesperidin and cinnamaldehyde in Jiubiying Weitong tablets was established.Results：（1）The powder of Jiubiying Weitong tablets showed the same microscopic characteristics with the reference drug of Aucklandiae Radix,Ilicis Rotundae Cortex,Cinnamon Cortex,Citri Reticulatae Pericarpium and Alpinia officinarum Rhizoma in Microscopic identification.（2）In the study of TLC identification,the TLC of hesperidin and cinnamaldehyde,costunolide,dehydrocostuslactone was clear.Meanwhile the spots were well separated and the negative control had no interference.（3）The linear ranges of costunolide and dehydrocostunolide fell within the ranges of 0.894 4-44.72 μg·m L-1（r=0.999 3）and 0.857 6-42.88 μg·m L-1（r=0.999 3）;-1 The linear ranges of hesperiand cinnamaldehyde fell within the ranges of 1.901-142.6 μg·m L（r=0.999 2）and 1.578-78.92μg·m L-d1 in（r=0.999 0）.The average recoveries（n=6）were 100.8%（RSD=2.1%）for costunolide,101.2%（RSD=2.2%）for dehydrocostunolide,101.3%（RSD=2.7%）for hesperidin and 96.20%（RSD=2.8%）for cinnamaldehyde.In 13 batches of samples,The content of costunolide and dehydrocostunolide were 0.011 6-0.200 8 mg·tablet-1 and 0.084 9-0.221 9 mg·tablet-1,the cContent of nhessperidin and cinnamaldehyde were 0.711 7-1.232 0 mg·tablet-1 and 0.029 5-1.007 5 mg·tablet-1.onclusio：This study established and improved the microscopic identification,TLC qualitative methods,and the determination method of the four target components.The new methods are simple,reproducible,specific,and can be applied to control the quality efficiently.These methods also provide a reference standard for the quality control of Jiubiying Weitong tablets.