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期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nifdc.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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顶空气相色谱法同时测定人参总皂苷中10种树脂残留成分

Simultaneous determination of ten resin residues in total saponins of Panax Ginseng by headspace gas chromatography

作者(英文):
分类号:R917
出版年·卷·期(页码):2017,37 (9):1680-0
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立顶空-气相色谱法测定人参总皂苷中10种树脂残留成分的含量。方法:以10%的NN-二甲基甲酰胺为提取溶剂,采用顶空进样,毛细管柱气相色谱测定树脂残留成分。柱温为程序升温(起始温度为60℃,保持1 min,以0.3℃·min-1升至62℃,再以10℃·min-1升至140℃,保持5 min);进样口温度:220℃,检测器温度:250℃。FID检测器,载气为氮气,流速1 mL·min-1,分流比为10:1;顶空进样,顶空平衡温度90℃,平衡时间为30 min,定量环温度110℃,传输管温度130℃,进样量1 mL,低速振摇。结果: 10种有机溶剂残留物的峰面积与质浓度呈良好线性关系,正己烷、甲基环己烷、苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯和二乙烯苯的平均回收率分别为102.65%、100.96%、103.34%、104.69%、96.14%、96.83%、96.81%、103.78%、94.69%和102.64%,3批市售样品除检出残留物邻二甲苯(含量分别为1.51、1.18、1.48μg·g-1)外,其他9种残留成分未检出。结论:所建立的方法能够较好地对人参总皂苷中10种树脂残留物进行限度测定。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To develop a determination method of ten resin residues in total saponins of Panax Ginseng by headspace GC. Method: The sample was dissolved with 10% DMF and analyzed by headspace capillary gas chromatography. The temperature program for the column was as follows:initially heated at 60℃ for 1 min, rose to 62℃ at a speed of 0. 3℃·min-1; then rose to 140℃ at a speed of 10℃·min-1, lasting for 5 min. The inlet temperature was 220℃ and FID detector temperature was set at 250℃. The split ratio was 10:1 and the flow rate of the carrier gas(N2)was 1 mL·min-1. Headspace conditions were as follows:the temperature and the time of balance for the sample were 90℃ and 30 min; the temperature of quantitative loop and transfer lines was 110℃ and 130℃. The sample volume was 1 mL, with low-speed shaking. Result: Linear relations between peak area and concentration of ten residues were good, average recoveries of n-hexane, hexahydrotoluene, benzene, methylbenzene, p-xylene, m-xylene, o-xylene, styrene, 1, 2-diethylbenzene and divinylbenzene were 102. 65%, 100. 96%, 103. 34%, 104. 69%, 96. 14%, 96. 83%, 96. 81%, 103. 78%, 94. 69% and 102. 64%, respectively. O-xylene was detected in three batches of samples from market(the content was 1. 51, 1. 18 and 1. 48 μg·g-1, respectively), and the other nine residues were not found in the samples. Conclusion: The method was suitable for detecting ten resin residues in total saponins of Panax Ginseng.

-----参考文献:---------------------------------------------------------------------------------------

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