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摘 要 目的：比較水蒸气蒸馏法（SD）与提取-共沸精馏耦合技术（WER）提取枳壳、香附总挥发油的效果，确定更优提取方法，以改善气滞胃痛颗粒剂中挥发性成分的提取工艺。方法：分别采用SD法与WER法提取枳壳、香附的总挥发油，对两种方法所提取挥发油的得率进行配对t检验；采用气相色谱-质谱联用技术（GC-MS）对两种方法所提取总挥发油进行分析，明确其主要成分，并采用面积归一化法测定并比较主要成分的相对含量。GC-MS分析采用色谱柱为Agilent HP-5毛细管柱（30 m×0.25 mm，0.25 μm），进样口温度为250 ℃，载气为氮气，流速为1 mL/min，分流比为20 ∶ 1，进样量为2 μL，程序升温，电轰击离子源，电子轰击能量为70 eV，扫描范围质荷比范围为50～500。结果：WER法所提挥发油颜色更加清澈，品相优于SD法提取挥发油，总挥发油的平均得率显著高于SD法（1.78% vs. 1.48%，P<0.01）；WER法与SD法所提取总挥发油中分别含39、38个成分，共有成分为38个。其中，D-柠檬烯、香附子烯、香附烯酮和α-香附酮为枳壳、香附总挥发油的主要成分，这4个成分共分别约占总成分的73.40%（WER法）和68.46%（SD法）。结论：相比于SD法，WER法提取枳壳、香附总挥发油的品相更好、得率更高、有效成分的含量更高，更适用于气滞胃痛颗粒剂中挥发性成分的提取。
关键词 提取-共沸精馏耦合技术；水蒸气蒸馏法；气相色谱-质谱联用技术；枳壳；香附；挥发油
Comparison of the Extraction Effects of Two Methods on the Total Volatile Oil from Citrus aurantium and Cyperus rotundus in Qizhi Weitong Granule
ZHENG Peng1，ZHAO Zhao2，DUN Jiaying1，LI Jiajia1，LI Chunhua1（1. College of Pharmacy， Hebei University of TCM， Shijiazhuang 050090， China； 2. Hebei Provincial Library， Shijiazhuang 050011， China）
ABSTRACT OBJECTIVE： To compare the extraction effects of steam distillation method （SD） and extraction-azeotropic distillation coupling technology （WER） on the volatile oil from Citrus aurantium and Cyperus rotundus， so as to determine the suitable extraction method and improve the extraction technology of volatile components in Qizhi weitong granule. METHODS： SD and WER were used to extract the total volatile oil from C. aurantium and C. rotundus. t-test was conducted for the yield of volatile oil extracted by the two methods. GC-MS method was used to analyze the volatile oil， and the main components were determined. The relative content of main components was determined compared by area normalization method. GC-MS conditions included that Agilent HP-5 capillary column （30 m×0.25 mm ， 0.25 μm）， inlet temperature of 250 ℃， nitrogen as carrier gas， flow rate of 1 mL/min， split ratio of 20 ∶ 1， sample size of 2 μL， temperature programmed， electron bombardment， electron bombardment energy of 70 eV， scanning range of m/z 50-500. RESULTS： The appearance of volatile oil extracted by WER was more clear， with better product phase than that by SD. The average yield of volatile oil extracted by WER method were significantly higher than SD method （1.78% vs. 1.48%， P<0.01）. The volatile oil extracted by WER method and SD method contained 39 and 38 components， involving 38 common components. Among them， D-limonene， acetophenone， ketoenone and α-ketone were the main components of the total volatile oil from C. aurantium and C. rotundus， and the sum of the 4 main components was about 73.40% （WER method） and 68.46% （SD method） of the total components. CONCLUSIONS： Compared with SD method， WER method for extracting volatile oil from C.aurantium and C. rotundus is better in product， phase higher in yield and higher in content of active volatiles， and is more suitable for the extraction of volatile components in Qizhi weitong granule.
关键词 提取-共沸精馏耦合技术；水蒸气蒸馏法；气相色谱-质谱联用技术；枳壳；香附；挥发油
Comparison of the Extraction Effects of Two Methods on the Total Volatile Oil from Citrus aurantium and Cyperus rotundus in Qizhi Weitong Granule
ZHENG Peng1，ZHAO Zhao2，DUN Jiaying1，LI Jiajia1，LI Chunhua1（1. College of Pharmacy， Hebei University of TCM， Shijiazhuang 050090， China； 2. Hebei Provincial Library， Shijiazhuang 050011， China）
ABSTRACT OBJECTIVE： To compare the extraction effects of steam distillation method （SD） and extraction-azeotropic distillation coupling technology （WER） on the volatile oil from Citrus aurantium and Cyperus rotundus， so as to determine the suitable extraction method and improve the extraction technology of volatile components in Qizhi weitong granule. METHODS： SD and WER were used to extract the total volatile oil from C. aurantium and C. rotundus. t-test was conducted for the yield of volatile oil extracted by the two methods. GC-MS method was used to analyze the volatile oil， and the main components were determined. The relative content of main components was determined compared by area normalization method. GC-MS conditions included that Agilent HP-5 capillary column （30 m×0.25 mm ， 0.25 μm）， inlet temperature of 250 ℃， nitrogen as carrier gas， flow rate of 1 mL/min， split ratio of 20 ∶ 1， sample size of 2 μL， temperature programmed， electron bombardment， electron bombardment energy of 70 eV， scanning range of m/z 50-500. RESULTS： The appearance of volatile oil extracted by WER was more clear， with better product phase than that by SD. The average yield of volatile oil extracted by WER method were significantly higher than SD method （1.78% vs. 1.48%， P<0.01）. The volatile oil extracted by WER method and SD method contained 39 and 38 components， involving 38 common components. Among them， D-limonene， acetophenone， ketoenone and α-ketone were the main components of the total volatile oil from C. aurantium and C. rotundus， and the sum of the 4 main components was about 73.40% （WER method） and 68.46% （SD method） of the total components. CONCLUSIONS： Compared with SD method， WER method for extracting volatile oil from C.aurantium and C. rotundus is better in product， phase higher in yield and higher in content of active volatiles， and is more suitable for the extraction of volatile components in Qizhi weitong granule.