摘要
目的 建立樟脑、薄荷脑、异龙脑、龙脑及水杨酸甲酯的气相含量测定方法及八角茴香、干姜、苍术、当归和山柰等药材的气相鉴别方法,并采用该方法对麝香壮骨膏进行质量分析。方法 色谱柱:DB-WAX、HP-5(30 m×0.32 mm,0.25 μm);分流比为10∶1和5∶1;载气流速均为1.0 mL·min^(-1);进样口温度220℃、检测器温度250℃,程序升温,进样量1 μL。结果 樟脑、薄荷脑、异龙脑、龙脑和水杨酸甲酯的线性范围分别为98.3~2840 ng、145.9~4216 ng、43.8~1267 ng、64.5~1863 ng、84.0~2427 ng(r=0.9999);精密度、重复性、稳定性的RSD均小于1.6%;平均加样回收率在94.52%~101.43%(RSD<2.6%)。196批样品中樟脑、薄荷脑、异龙脑、龙脑和水杨酸甲酯含量分别为0.420~60.786、4.251~89.129、0.717~25.876、1.664~36.014、1.536~40.452 mg/100 cm^(2)。196批麝香壮骨膏中,含量测定项47批不合格,气相鉴别项33批不合格。结论 本文建立的麝香壮骨膏气相色谱定量定性分析方法专属性及特征性强,且简便、快速、准确,为全面控制麝香壮骨膏质量提供了依据。
Objective To determine the content of camphor,menthol,isoborneol,borneol and methyl salicylate by gas chromatograph method and identify Anise stellati Fructus,Crude Zingber Officinale,Rhizoma Atractylodis,Angelica Sinensis and Kaempferia Galanga Linn.Methods The chromatographic separation was conducted on DB-WAX and HP-5 (30 m×0.32 mm,0.25 μm) column with temperature programming,at the flow rate of 1.0 mL·min^(-1).The split ratio was 10∶1 and 5∶1,the inlet temperature was set at 220℃,the detector temperature was set at 250℃,and the volume of sample injection was 1 μL.Results The linearity of camphor,menthol,isoborneol,borneol and methyl salicylate were 98.3~2840 ng,145.9~4216 ng,43.8~1267 ng,64.5~1863 ng,84.0~2427 ng (r=0.9999),respectively.The RSDs of precision,stability and reproducibility tests were all lower than 1.6%.The average recoveries were 94.52%~101.43% (RSD<2.6%).The contents of 196 batches of camphor,menthol,isoborneol,borneol and methyl salicylate ranged 0.420~60.786,4.251~89.129,0.717~25.876,1.664~36.014,and 1.536~40.452 mg/100 cm^(2).In the 196 batches of Shexiang Zhuanggu plaster,content determination items in 47 batches were unqualified,and those in 33 batches of GC identification were unqualified.Conclusion The proposed method of content determination and chromatogram analysis has specificity and strong characterstics.This method is easy,fast and reliable,and can be used for the quality control of the preparation.
作者
许苗苗
张楠
谢志民
XU Miao-miao;ZHANG Nan;XIE Zhi-min(Xi’an Municipal Institute for Food and Drug Control,Xi’an 710054)
出处
《中南药学》
CAS
2022年第11期2606-2610,共5页
Central South Pharmacy
基金
2021年国家药品评价性抽验中央补助地方经费项目(No.111)。
关键词
气相色谱法
麝香壮骨膏
樟脑
薄荷脑
冰片
gas chromatograph
Shexiang Zhuanggu plaster
camphor
menthol
borneol
