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作 者:周文杰 饶伟文 王丽丽 ZHOU Wenjie;RAO Weiwen;WANG Lili(Guilin Food and Drug Inspection Institute,Guilin,Guangxi,China 541012)
机构地区:[1]广西壮族自治区桂林市食品药品检验所,广西桂林541012
出 处:《中国药业》2023年第3期80-83,共4页China Pharmaceuticals
摘 要:目的建立枫香精油的质量标准。方法从性状特征、薄层色谱方面对枫香精油进行定性鉴别。按2020年版《中国药典(四部)》方法测定枫香精油的相对密度和折光率,按《香料酸值或含酸量的测定》GB/T 14455.5—2008测定酸值。采用气相色谱-质谱(GC-MS)法分离、鉴定枫香精油的化学成分,色谱柱为DB-5MS毛细管柱(30 m×250μm,0.25μm),载气为氦气,分流比为100∶1,体积流量为1.0 mL/min,进样口温度为250℃,辅助加热区温度为280℃,程序升温,进样量为0.1μL;离子源为电子轰击(EI),离子源温度为230℃,四极杆温度为150℃,电子能量为70 eV,扫描范围为20~450 amu(全扫)。采用峰面积归一化法测定主要特征成分的相对含量。结果16批制剂均为淡黄色澄清液体,气芳香;薄层色谱图与枫香脂对照药材在相应位置显相同颜色的斑点,且斑点清晰,分离良好;相对密度(20℃)为0.910~0.924,折光率(20℃)为1.493~1.500,酸值为10.08~18.30 mg/g;含有39种化合物,β-石竹烯、α-蒎烯、β-蒎烯、莰烯为主要特征成分,相对含量分别为27.14%~36.53%,10.65%~17.32%,6.71%~12.44%,1.17%~6.27%。结论所建立的方法可用于枫香精油的质量控制。Objective To establish the quality standard of Liquidambaris Resina Essential Oil.Methods The characteristics analysis and the thin-layer chromatography(TLC)method were used for the qualitative identification of Liquidambaris Resina Essential Oil.The relative density and refractive index of Liquidambaris Resina Essential Oil were determined according to the method of the Chinese Pharmacopoeia(2020 Edition,VolumeⅣ),and the acid value was determined according to the method of the Fragrance/Flavor Substance—Determination of Acid Value or Acid Content(GB/T 14455.5—2008).The chemical components of Liquidambaris Resina Essential Oil were separated and identified by the gas chromatography-mass spectrometry(GC-MS)method.The chromatographic column was DB-5MS capillary column(30 m×250μm,0.25μm),the carrier gas was helium,the split ratio was 100∶1,the volume flow was 1.0 mL/min,the inlet temperature was 250℃,the temperature of the auxiliary heating zone was 280℃,the temperature was programmed,and the injection volume was 0.1μL.The ion source was electron impact(EI),the ion source temperature was 230℃,the quadrupole temperature was 150℃,the electron energy was 70 eV,and the scanning range was 20-450 amu(full scan).The relative contents of main characteristic components were determined by the peak area normalization method.Results The 16 batches of preparations were all light-yellow and clear liquid with aroma.The TLC chromatograms showed that there were spots with the same color at the corresponding positions as the Liquidambaris Resina reference,and the spots were clear and well separated.The relative density of the preparation(at the temperature of 20℃)was in the range of 0.910-0.924,the refractive index(at the temperature of 20℃)was in the range of 1.493-1.500,and the acid value was in the range of 10.08-18.30 mg/g.There were 39 compounds in the preparation,among them,β-caryophyllene,α-pinene,β-pinene and camphene were the main characteristic components with the relative contents of 27.14%-36.53
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