正交实验设计优选薄荷芳香水的提取工艺
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摘要
以薄荷为试材,建立气相色谱(GC)测定薄荷芳香水中薄荷脑含量的方法,色谱柱选择5%苯基-甲基聚硅氧烷为固定液的毛细管柱(30m×0.32mm×0.25μm);载气为氮气,流速1.5mL·min~(-1),氢气流速40mL·min~(-1);检测器温度280℃;进样口温度250℃;进样量为1μL。采用水蒸气蒸馏法提取薄荷芳香水,以挥发油提取量和薄荷脑含量为考核指标,以加水量、药材浸泡时间和提取时间为考察因素,进行L9(34)正交实验,优选薄荷芳香水的提取工艺。结果表明:采用GC测定薄荷芳香水中薄荷脑的含量,薄荷脑浓度在0.02～0.20mg·mL~(-1)线性关系良好(r=0.999 8),准确度、精密度RSD均小于5%,色谱条件发生小的变动不会影响测定结果。正交实验结果表明,浸泡时间是影响薄荷挥发油提取的主要因素,其次为提取时间、加水量;最佳提取工艺为加8倍量水,浸泡1.5h,提取3.0h。
Taking Mentha haplocalyxas test material to study the extraction of volatile oil in Mentha haplocalyx by orthogonal experimental design.GC method was established to determine the contents of menthol.Gas chromatography(GC)was performed on the column of Agilent HP-5 capillary column(30 m ×0.32 mm ×0.25μm).Nitrogen gas was used as carrier gas,and the flow rate was 1.5 mL·min~(-1).The flow rate of hydrogen was 40 mL· min~(-1).The detection temperature was 280℃.The injection temperature was 250 ℃.The injection volume was 1 μL.Volatile oil was extracted by steam distillation.Initial amount of solvent,soaking time,extraction time were examined by taking the volatile oil extraction amount and menthol content as the evaluation index.The preparation process was optimized by L_9(3~4)orthogonal experimental design.The GC method was feasible and accurate for the determination of menthol in the volatile oil.The linear range was 0.02-0.20mg·mL~(-1)(r=0.999 8),and RSDs of precision and accuracy tests were all lower than 5%.Soaking time was the key factor influencing the extraction of volatile oil.The optimal preparation for volatile oil were adding initial amount of water by 8 times,soaking for 1.5 hours and eatracting for 3.0 hours.
Taking Mentha haplocalyxas test material to study the extraction of volatile oil in Mentha haplocalyx by orthogonal experimental design.GC method was established to determine the contents of menthol.Gas chromatography(GC)was performed on the column of Agilent HP-5 capillary column(30 m ×0.32 mm ×0.25μm).Nitrogen gas was used as carrier gas,and the flow rate was 1.5 mL·min~(-1).The flow rate of hydrogen was 40 mL· min~(-1).The detection temperature was 280℃.The injection temperature was 250 ℃.The injection volume was 1 μL.Volatile oil was extracted by steam distillation.Initial amount of solvent,soaking time,extraction time were examined by taking the volatile oil extraction amount and menthol content as the evaluation index.The preparation process was optimized by L_9(3~4)orthogonal experimental design.The GC method was feasible and accurate for the determination of menthol in the volatile oil.The linear range was 0.02-0.20mg·mL~(-1)(r=0.999 8),and RSDs of precision and accuracy tests were all lower than 5%.Soaking time was the key factor influencing the extraction of volatile oil.The optimal preparation for volatile oil were adding initial amount of water by 8 times,soaking for 1.5 hours and eatracting for 3.0 hours.
引文
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[12]柴鑫莉,祝春仙,姜玲丽,等.顶空气相色谱法测定市售56批次强力枇杷露中薄荷脑的含量[J].中国药房,2015,29(30):4288-4290.
[13]蔡薇,廖锡锵.伤科黄水消除胫腓骨双骨折术前肿胀疗效观察[J].亚太传统医药,2017,13(2):140-141.
[14]潘海文,王朝辉,李卓伟,等.伤科黄水预防断指再植术后血管危象的临床观察[J].中成药,2017,39(5):916-921.
[15]罗学辉,谢学文,曾文磊,等.关节镜下有限清理术配合伤科黄水外敷治疗膝骨性关节炎的效果[J].广东医学,2016,37(7):1078-1081.
[2]张援虎,刘颖,胡峻,等.薄荷中黄酮类成分的研究[J].中草药,2006,37(4):512-514.
[3]曾建伟,钱士辉,吴锦忠,等.薄荷非挥发性成分研究[J].中国中药杂志,2006,31(5):400-402.
[4]刘颖,张援虎,石任兵.薄荷化学成分的研究[J].中国中药杂志,2005,30(14):1086-1088.
[5]彭蕴茹,钱士辉,石磊,等.薄荷非挥发性提取部位的药理活性研究[J].中药材,2008,31(1):104-107.
[6]吕乔璐,武维,迟森森,等.HS/SPME-GC-MS法分析不同采收期薄荷药材挥发油成分动态变化[J].北京中医药大学学报,2017,40(2):155-158.
[7]张小飞,万娜,詹娟娟,等.Box-Behnken响应面法优化江西产薄荷挥发油提取工艺及其动力学研究[J].辽宁中医药大学学报,2016,18(5):65-69.
[8]迟玉广,李中阳,黄爱华,等.不同产地薄荷饮片中挥发性成分的比较分析[J].安徽医药,2016,20(9):1661-1664.
[9]张璐,田静.复方薄荷脑醑的质量标准研究[J].中药材,2017,40(2):399-401.
[10]张群,蔡晓翠,贺金华.气相色谱法测定复方薰衣草油膏中薄荷脑的含量[J].中国医院用药评价与分析,2017,17(5):604-605,608.
[11]董村,赵宇,王赫男.GC法测定出口京万红软膏中薄荷脑的含量[J].中华中医药杂志,2016,31(6):2404-2405.
[12]柴鑫莉,祝春仙,姜玲丽,等.顶空气相色谱法测定市售56批次强力枇杷露中薄荷脑的含量[J].中国药房,2015,29(30):4288-4290.
[13]蔡薇,廖锡锵.伤科黄水消除胫腓骨双骨折术前肿胀疗效观察[J].亚太传统医药,2017,13(2):140-141.
[14]潘海文,王朝辉,李卓伟,等.伤科黄水预防断指再植术后血管危象的临床观察[J].中成药,2017,39(5):916-921.
[15]罗学辉,谢学文,曾文磊,等.关节镜下有限清理术配合伤科黄水外敷治疗膝骨性关节炎的效果[J].广东医学,2016,37(7):1078-1081.