不同剂量~(60)Co-γ射线辐照对小儿感冒颗粒挥发性成分的影响
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摘要
目的:建立气相色谱法同时测定小儿感冒颗粒中α-蒎烯、β-蒎烯、薄荷脑、百秋李醇和广藿香酮5个挥发性成分的含量,考察不同剂量~(60)Co-γ射线辐照前后挥发性成分的变化。方法:采用Agilent HP-5MS(30 m×0.32 mm×0.25μm)色谱柱,柱温采用程序升温,进样口温度220℃,检测器温度250℃,分流比为30:1,检测器为氢火焰离子化检测器,载气为氮气,流速为1.5 mL·min~(-1),进样量为1μL。分别选择2、5、8 kGy的辐照剂量对小儿感冒颗粒进行辐照,比较辐照前后小儿感冒颗粒中5个挥发性成分含量的变化,并进行成组t检验考察其显著情况。结果:百秋李醇、广藿香酮、α-蒎烯、β-蒎烯及薄荷脑进样量分别在0.011 38～0.568 8、0.018 84～0.941 9、0.010 97～0.548 5、0.017 58～0.879 0及0.020 86～1.043 1μg范围内有良好线性,平均加样回收率分别为101.8%、100.9%、99.7%、98.9%和100.5%,RSD分别为1.3%、1.1%、0.90%、1.0%和1.2%。经过2、5、8 kGy辐照后,小儿感冒颗粒所含的挥发性成分α-蒎烯、β-蒎烯、薄荷脑、百秋李醇和广藿香酮均有变化,经成组t检验,在超过5 kGy后,α-蒎烯辐照前后含量变化显著(P<0.05)。结论:所建立的小儿感冒颗粒挥发性成分测定方法回收率高,重复性好,灵敏度高,可作为小儿感冒颗粒质控方法。在辐照剂量不超过5 kGy时,各挥发性成分变化不显著,可为小儿感冒颗粒辐照灭菌手段提供参考。
Objective:To establish a GC method for simultaneous determination of 5 volatile components(patchoulialcohol,pogostone,α-pinene,β-pinene and menthol)in children cold granules and to study the effects of ~(60)Co-γ ray irradiation on the volatile components of children cold granules.Methods:The capillary column Agilent HP-5 MS(30 m×0.32 mm×0.25 μm)was adopted and the column temperature was controlled by programming,the injector temperature was 220 ℃ and the detector temperature was 250 ℃.The split ratio was30∶1 and the injection volumn was 1 μL.The detector was a hydrogen flame ionization detector,the carrier gas was nitrogen and the flow rate was 1.5 mL·min~(-1).Content of the 5 volatile components before and after irradiation at doses of 2,5 and 8 kGy were compared,and a t test study was used to examine the significant condition. Results:The linear range of patchoulialcohol,pogostone,α-pinene,β-pinene and menthol were 0.011 38-0.568 8,0.018 84-0.941 9,0.010 97-0.548 5,0.017 58-0.879 0 and 0.020 86-1.043 1 μg,and the average recoveries were 101.8%,100.9%,99.7%,98.9% and 100.5% with RSDs of 1.3%,1.1%,0.90%,1.0% and1.2%.After irradiation at doses of 2,5,8 kGy,patchoulialcohol,pogostone,α-pinene,β-pinene and menthol varied.By group t-test,content of α-pinene varied significantly(P<0.05)before and after irradiation at doses over5 kGy.Conclusion:The established method has high recovery rate,good repeatability and high sensitivity,can be used for quality control of children cold granules.When the radiation dose is not more than 5 kGy,the changes of each volatile components are not significant,which can provide a reference for the sterilization of children cold granules.
Objective:To establish a GC method for simultaneous determination of 5 volatile components(patchoulialcohol,pogostone,α-pinene,β-pinene and menthol)in children cold granules and to study the effects of ~(60)Co-γ ray irradiation on the volatile components of children cold granules.Methods:The capillary column Agilent HP-5 MS(30 m×0.32 mm×0.25 μm)was adopted and the column temperature was controlled by programming,the injector temperature was 220 ℃ and the detector temperature was 250 ℃.The split ratio was30∶1 and the injection volumn was 1 μL.The detector was a hydrogen flame ionization detector,the carrier gas was nitrogen and the flow rate was 1.5 mL·min~(-1).Content of the 5 volatile components before and after irradiation at doses of 2,5 and 8 kGy were compared,and a t test study was used to examine the significant condition. Results:The linear range of patchoulialcohol,pogostone,α-pinene,β-pinene and menthol were 0.011 38-0.568 8,0.018 84-0.941 9,0.010 97-0.548 5,0.017 58-0.879 0 and 0.020 86-1.043 1 μg,and the average recoveries were 101.8%,100.9%,99.7%,98.9% and 100.5% with RSDs of 1.3%,1.1%,0.90%,1.0% and1.2%.After irradiation at doses of 2,5,8 kGy,patchoulialcohol,pogostone,α-pinene,β-pinene and menthol varied.By group t-test,content of α-pinene varied significantly(P<0.05)before and after irradiation at doses over5 kGy.Conclusion:The established method has high recovery rate,good repeatability and high sensitivity,can be used for quality control of children cold granules.When the radiation dose is not more than 5 kGy,the changes of each volatile components are not significant,which can provide a reference for the sterilization of children cold granules.
引文
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[11]张小龙,孙晓,马新飞,等.气相色谱法同时测定小儿感冒颗粒中百秋李醇、薄荷脑、α-蒎烯、β-蒎烯的含量[J].首都食品与医药,2014(22):110ZHANG XL,SUN X,MA XF,et al.Simultaneous determination of the content of patchoulialc chol,menthol,alpha pinene and beta pinene in infantile cold particles by gas chromatography[J].Capit Food Med,2014(22):110
[12]徐国兵.GC法同时测定复方麝香注射液中薄荷脑、龙脑、百秋李醇和麝香酮的含量[J].中成药,2008,30(6):855XU GB.Simultaneous determination of menthol,borneol,patchouli alcohol and Muscone in compound musk injection by GC[J].Chin Tradit Pat Med,2008,30(6):855
[13]刘玉红,李青苗,黄志芳,等.GC法测定鱼腥草挥发油中α-蒎烯、β-蒎烯等7种成分的含量[J].药物分析杂志,2015,39(10):1810LIU YH,LI QM,HUANG ZF,et al.GC determination of the content of alpha pinene and beta pinene in the volatile oil of Houttuynia cordata Houttuyniae and other 7 components[J].Chin J Pharm Anal,2015,39(10):1810
[14]严永亮.α-蒎烯物理、化学性质及其应用[J].中国化工贸易,2015,7(24):2YAN YL,Alpha pinene physical,chemical properties and applications[J].China Chemi trade,2015,7(24):2
[15]熊德元,莫炳荣,黄科林,等.α-蒎烯-β-蒎烯共聚物的热稳定性与热降解动力学[J].广西大学学报(自然科学版),2009,34(2):168XIONG DY,MO BR,HUANG KL,et al.Thermal stability and thermal degradation kinetics of alpha pinene-beta-pinene copolymer[J].J Guangxi Univ(Nat Sci Ed),2009,34(2):168
[2]张立雯,林玲,林彤,等.龙胆和秦艽钴60辐照前后指纹图谱变化的研究[J].药物分析杂志,2015(12):2173ZHANG LW,LIN L,LIN T,et al.Study on the changes of fingerprints of gentiana and gentiana macrophylla cobalt 60 before and after irradiation[J].Chin J Pharm Anal,2015(12):2173
[3]吴柯,赵冠人,陈明,等.钴60γ射线辐射对异烟肼稳定性的影响[J].中国药师,2017,(11):2064WU K,ZHAO GR,CHEN M,et al.Effects of cobalt 60 gamma ray irradiation on isoniazid stability[J].China Pharm,2017,(11):2064
[4]中华人民共和国药典2015年版.一部[S].2015:560ChP 2015.VolⅠ[S].2015:560
[5]徐雯,吴燕青,丁浩然,等.广藿香的药理作用及机制研究进展[J].上海中医药杂志,2017(10):103XU W,WU YQ,DING HR,et al.Progress in pharmacological action and mechanism of patchouli[J].Shanghai J Tradit Chin Med,2017(10):103
[6]王吉春.广藿香中挥发油成分的研究进展[J].中国医药指南,2010,8(11):43WANG JC.Advances in the research of volatile oil from patchouli[J].Chin Med Guide,2010,8(11):43
[7]魏晋宝,杨光义,陈欢,等.连翘苷的提取方法、药理毒理及药动学研究进展[J].中国药师,2015(12):2144WEI JB,YANG GY,CHEN H,et al.Progress in extraction,pharmacology,toxicology and pharmacokinetics of forsythin[J].China Pharm,2015(12):2144
[8]郭丁丁.中药连翘挥发油成分及提取方法的研究进展[J].山西中医学院学报,2013,14(1):73GUO DD.Research progress on constituents and extraction methods of volatile oil from Forsythia suspense[J].J Shanxi Univ Tradit Chin Med,2013,14(1):73
[9]程丽萍,郇瑜,赵洪雨,等.GC法测定甘油止痒洗剂中苯酚和薄荷脑的含量[J].中国药师.2014,16(11):1815CHENG LP,YU Y,ZHAO HY,et al.Determination of phenol and menthol in glycerin antipruritic lotion by GC[J].China Pharm,2014,16(11):1815
[10]于夏,刘超,崔雪靖,等.3种河南产薄荷挥发性成分分析[J].中国实验方剂学杂志.2014,20(21):87[10]YU X,LIU C,CUI XJ,et al.Analysis of volatile constituents of 3kinds of mint produced in Henan[J].Chin J Exp Tradit Med Form,2014,20(21):87
[11]张小龙,孙晓,马新飞,等.气相色谱法同时测定小儿感冒颗粒中百秋李醇、薄荷脑、α-蒎烯、β-蒎烯的含量[J].首都食品与医药,2014(22):110ZHANG XL,SUN X,MA XF,et al.Simultaneous determination of the content of patchoulialc chol,menthol,alpha pinene and beta pinene in infantile cold particles by gas chromatography[J].Capit Food Med,2014(22):110
[12]徐国兵.GC法同时测定复方麝香注射液中薄荷脑、龙脑、百秋李醇和麝香酮的含量[J].中成药,2008,30(6):855XU GB.Simultaneous determination of menthol,borneol,patchouli alcohol and Muscone in compound musk injection by GC[J].Chin Tradit Pat Med,2008,30(6):855
[13]刘玉红,李青苗,黄志芳,等.GC法测定鱼腥草挥发油中α-蒎烯、β-蒎烯等7种成分的含量[J].药物分析杂志,2015,39(10):1810LIU YH,LI QM,HUANG ZF,et al.GC determination of the content of alpha pinene and beta pinene in the volatile oil of Houttuynia cordata Houttuyniae and other 7 components[J].Chin J Pharm Anal,2015,39(10):1810
[14]严永亮.α-蒎烯物理、化学性质及其应用[J].中国化工贸易,2015,7(24):2YAN YL,Alpha pinene physical,chemical properties and applications[J].China Chemi trade,2015,7(24):2
[15]熊德元,莫炳荣,黄科林,等.α-蒎烯-β-蒎烯共聚物的热稳定性与热降解动力学[J].广西大学学报(自然科学版),2009,34(2):168XIONG DY,MO BR,HUANG KL,et al.Thermal stability and thermal degradation kinetics of alpha pinene-beta-pinene copolymer[J].J Guangxi Univ(Nat Sci Ed),2009,34(2):168