气相色谱-质谱研究加味逍遥丸中的挥发性成分
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摘要
目的:基于气相色谱-质谱研究方法检测分析加味逍遥丸中的挥发性成分。方法:首先采用水蒸气蒸馏法提取加味逍遥丸供试品溶液中的挥发性成分,以正十八烷为内标物进行参照,通过正交试验设计研究,将提取时间9 h、固液比1∶15、浸泡时间10 h时是水蒸馏法提取加味逍遥丸中挥发性成分的最佳提取条件,进一步分析加味逍遥丸中挥发性成分的气相色谱-质谱图及具体化学成分,GC-MS色谱质谱研究方法色谱条件:选择直径为0. 25μm的Rxi-5ms的色谱柱(规格:30m×0. 25 mm),柱流量为1 m L/min;以氦气(He)为载气,采用30∶1的分流比;进样量:0. 5μL,以260℃为进样口温度,升温程序:首先保持初始柱温60℃3 min,随后以10℃/min的升温速率升至175℃,再下降10倍升温速率以1℃/min缓慢升温至195℃,最后增加5倍升温速率以5℃/min升温至240℃,维持15 min后再缓慢升至250℃的接口温度;溶剂延迟时间为3 min。质谱条件:电子轰击离子源的轰击能量设置为70 e V,离子源温度设置为200℃;以0. 7KV为检测电压;采用全谱扫描,其质量扫描范围为m/z 40～550 amu。结果:气相色谱-质谱研究方法严谨性精密度、重复性和稳定性试验结果均良好。加味逍遥丸在气相色谱-质谱研究中以正十八烷(S)为内标物,检测到53中挥发性成分。将总离子流色谱图中所检测出的色谱峰与NIST标准质谱数据库中的标准谱图进行参照比较,分析53个挥发性成分的具体化学成分信息,其中芳香族类和萜烯类挥发性成分均有11种,萜醇类挥发性成分有8中种,醛类挥发性成分有6种。结论:气相色谱-质谱方法研究加味逍遥丸中挥发性物质,分析其具体化学成分,为加味逍遥丸的质量控制提供依据。
Objective: To detect the volatile components in Modified Xiaoyao Pills by gas chromatography mass spectrometry.Methods: The volatile components in the solution of Modified Xiaoyao Pills were extracted by steam distillation. N-octadecane was used as internal standard substance for reference. Through the design of the orthogonal experiment,it was found that when the extraction time was 9 hours,the solid-liquid ratio was 1∶ 15,and the soaking time was 10 hours,it was the best time to extract the volatile components in Modified Xiaoyao Pills by water distillation. The gas chromatography-mass spectrum and the specific chemical components of volatile components in Modified Xiaoyao Pills were analyzed. The chromatography condition of GC-MS chromatogram mass spectrometric study: the Rxi-5 ms chromatographic column( 30 m × 0. 25 mm) was selected,the column flow rate was 1 m L/min; the flow ratio of helium gas( He) was used as the carrier gas,and the flow ratio of 30: 1 was adopted; the sample volume was0. 5 μL,the inlet temperature was 260 ℃. The temperature rising procedure started. First the temperature of the initial column temperature was 60 ℃ for 3 minutes,the temperature rose to 175 ℃ by the heating rate of 10 ℃/min,and decreased by 10 times at the rate of 1 ℃/min to 195 ℃,and at last increased the heating rate 5 times to 240 ℃ at the rate of 5 ℃/min,and then slowly increased to 250 ℃ after 15 minutes,and the delay time of solvent was 3 minutes. Mass spectrum condition: the bombardment energy of the electronic bombardment ion source was set to 70 eV,the temperature of the ion source was set to 200 c,and the voltage was detected by 0. 7 KV; the scanning range of the total spectrum was m/z40-550 amu. Results: The accuracy,repeatability and stability of the GC-MS method were good. In the GC-MS study,N-octadecane( S) was used as the internal standard substance in Modified Xiaoyao Pills to detect the volatile components in 53. By comparing the chromatographic peaks detected in the total ion flow chromatogram with the standard spectra of NIST standard mass spectrometry database,the specific chemical composition information of the 53 volatile components was analyzed,including 11 aromatic and terpene volatile components,8 species of terpene alcohols and 6 kinds of aldehydes. Conclusion: Gas chromatography-mass spectrometry( GC-MS) is used to study the volatile substances in Modified Xiaoyao Pills,and to analyze its specific chemical composition and provide the basis for the quality control of Modified Xiaoyao Pills.
Objective: To detect the volatile components in Modified Xiaoyao Pills by gas chromatography mass spectrometry.Methods: The volatile components in the solution of Modified Xiaoyao Pills were extracted by steam distillation. N-octadecane was used as internal standard substance for reference. Through the design of the orthogonal experiment,it was found that when the extraction time was 9 hours,the solid-liquid ratio was 1∶ 15,and the soaking time was 10 hours,it was the best time to extract the volatile components in Modified Xiaoyao Pills by water distillation. The gas chromatography-mass spectrum and the specific chemical components of volatile components in Modified Xiaoyao Pills were analyzed. The chromatography condition of GC-MS chromatogram mass spectrometric study: the Rxi-5 ms chromatographic column( 30 m × 0. 25 mm) was selected,the column flow rate was 1 m L/min; the flow ratio of helium gas( He) was used as the carrier gas,and the flow ratio of 30: 1 was adopted; the sample volume was0. 5 μL,the inlet temperature was 260 ℃. The temperature rising procedure started. First the temperature of the initial column temperature was 60 ℃ for 3 minutes,the temperature rose to 175 ℃ by the heating rate of 10 ℃/min,and decreased by 10 times at the rate of 1 ℃/min to 195 ℃,and at last increased the heating rate 5 times to 240 ℃ at the rate of 5 ℃/min,and then slowly increased to 250 ℃ after 15 minutes,and the delay time of solvent was 3 minutes. Mass spectrum condition: the bombardment energy of the electronic bombardment ion source was set to 70 eV,the temperature of the ion source was set to 200 c,and the voltage was detected by 0. 7 KV; the scanning range of the total spectrum was m/z40-550 amu. Results: The accuracy,repeatability and stability of the GC-MS method were good. In the GC-MS study,N-octadecane( S) was used as the internal standard substance in Modified Xiaoyao Pills to detect the volatile components in 53. By comparing the chromatographic peaks detected in the total ion flow chromatogram with the standard spectra of NIST standard mass spectrometry database,the specific chemical composition information of the 53 volatile components was analyzed,including 11 aromatic and terpene volatile components,8 species of terpene alcohols and 6 kinds of aldehydes. Conclusion: Gas chromatography-mass spectrometry( GC-MS) is used to study the volatile substances in Modified Xiaoyao Pills,and to analyze its specific chemical composition and provide the basis for the quality control of Modified Xiaoyao Pills.
引文
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[2]古丽巴哈尔·托乎提,艾山·艾比布勒,杨玲玲,等.加味逍遥丸微生物适用性试验方法与评价[J].食品安全质量检测学报,2018,9(1):178-183.
[3]龚彦溶,谭志滨,王术玲.10种中药制剂中柴胡的定量测定[J].中成药,2017,39(6):1305-1308.
[4]石勇强.加味逍遥丸的制备与质量控制[J].医学信息(中旬刊),2011,24(1):335-337.
[5]陈帅,王磊,高双,等.HPLC-DAD法同时测定加味逍遥丸中8种成分[J].中草药,2016,47(21):3829-3833.
[6]陈玉杰.高效毛细管电泳法测定加味逍遥丸中芍药苷、栀子苷的含量[J].中国实验方剂学杂志,2012,18(10):146-149.
[7]任红心.RP-HPLC法测定加味逍遥丸中栀子苷的含量[J].中医研究,2012,25(5):71-73.
[8]黄翼飞,蔡赞,胡静,等.气相色谱-红外光谱联用技术及应用研究进展[J].光谱学与光谱分析,2015,20(8):2130-2135.
[9]李雪,王倩倩,徐晨,等.中药质谱分析方法及应用研究[J].中国科学:化学,2014,31(5):701-709.
[10]陈佳,钱琛,陈桂良.《中华人民共和国药典(2015年版)》中中药部分的增、修订情况简介[J].上海医药,2016,37(7):3-4,8.
[11]高立新.气相色谱-质谱联用技术在药物分析中的应用[J].中外医疗,2014,33(5):190-191.
[12]陈智煌,廖华军,刘晨,等.羌活挥发油的GC-MS分析及其抗炎镇痛的药理作用初探[J].海峡药学,2015,17(08):20-23.
[13]薛子钰,华永丽,李锦霞,等.当归不同炮制品挥发油给药大鼠的尿液代谢组学研究[J].中国中药杂志,2016,41(5):928-939.
[14]于赟,陈川.中药挥发油提取技术及生物活性的研究进展[J].上海中医药大学学报,2014,27(2):75-78.
[15]傅瑶,李颜,霍炎,等.铁线莲属植物中挥发性成分的研究进展[J].中国药房,2013,73(11):1047-1049.
[16]梁悦,王璐,茹鑫,等.逍遥丸(水丸)挥发性成分的提取及其气相色谱-质谱法分析[J].分析测试学报,2009,28(10):1170-1175.
[17]贾科雷,刘维海.正交设计优化加味逍遥丸塑制法生产工艺[J].现代中医药,2011,31(1):63-64.
[18]邱美贤.逍遥散复方配伍颗粒质量标准规范化研究[D].广州:广州中医药大学,2006.