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活血消痛酊挥发性成分的鉴定及含量测定

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目的 建立鉴定活血消痛酊中挥发性成分及测定其中 5 种指标性成分含量的气相色谱-质谱联用(GC-MS)法。方法 色谱柱为Agilent PEG20M毛细管柱(30 m×0。32 mm,0。25 μm),程序升温,进样口温度为 230℃,载气为高纯氦气,流速为 1。0 mL/min,分流比为 5∶1(V/V),进样量为 1 μL;采用电子轰击离子源(成分鉴定)或选择性离子监测模式(含量测定),质量扫描范围为m/z 40~500。结果 共鉴定出 37 种挥发性成分。3-蒈烯、桉油精、β-石竹烯、丁香酚、对甲氧基肉桂酸乙酯的质量浓度分别在0。200 2~40。04 μg/mL、0。202 6~40。52 μg/mL、0。299 2~59。84 μg/mL、0。601 0~120。20 μg/mL、0。302 2~60。44 μg/mL范围内与待测成分离子强度线性关系良好(R2>0。999 0,n=7);检测限分别为 3。11,2。94,3。29,7。58,4。35 ng/mL,定量限分别为 10。31,9。75,10。90,25。03,14。49 ng/mL;精密度、稳定性、重复性试验结果的RSD均小于 5%(n=6);平均加样回收率分别为 93。01%,91。90%,94。69%,93。42%,92。70%,RSD分别为 4。98%,5。53%,5。04%,4。29%,4。83%(n=9)。20 批样品中,上述 5 种成分的平均含量分别为1。48,2。07,3。26,8。80,3。59 μg/mL。结论 该方法操作简便,结果准确,重复性好,可用于活血消痛酊挥发性成分的鉴定及含量测定。
Identification and Content Determination of Volatile Components in Huoxue Xiaotong Tincture
Objective To establish a gas chromatography-mass spectrometry(GC-MS)method for identifying the volatile components in Huoxue Xiaotong Tincture and determining the contents of five indicator components.Methods The chromatographic column was the Agilent PEG20M capillary column(30 m×0.32 mm,0.25 μm),the temperature was programmed,the inlet temperature was 230℃,the carrier gas was high-purity helium,the flow rate was 1.0 mL/min,the split ratio was 5∶1(V/V),and the injection volume was 1 μL.The electron impact ion source(component identification)or selective ion monitoring mode(content determination)was adopted,the mass scanning range was m/z 40-500.Results A total of 37 volatile components were identified.The linear ranges of 3-carene,cineole,β-caryophyllene,eugenol and ethyl p-methoxycinnamate were 0.200 2-40.04 μg/mL,0.202 6-40.52 μg/mL,0.299 2-59.84 μg/mL,0.601 0-120.20 μg/mL,0.302 2-60.44 μg/mL(R2>0.999 0,n=7)respectively.The limits of detection(LOD)of the above five components were 3.11,2.94,3.29,7.58,4.35 ng/mL,and their limits of quantification(LOQ)were 10.31,9.75,10.90,25.03,14.49 ng/mL respectively.The RSDsof precision,stability,repeatability tests were all lower than 5%(n=6).The recovery rates of the above five components were 93.01%,91.90%,94.69%,93.42%.92.70%,with RSDs of 4.98%,5.53%,5.04%,4.29%,4.83%,respectively(n=9).Among the 20 batches of samples,the average contents of 3-carene,cineole,β-caryophyllene,eugenol and ethyl p-methoxycinnamate were 1.48,2.07,3.26,8.80,3.59 μg/mL respectively.Conclusion This method is simple,accurate and repeatable,which can be used for the identification and content determination of volatile components in Huoxue Xiaotong Tincture.

Huoxue Xiaotong Tincturevolatile componentGC-MScomponent identificationcontent determination

方强、郭立、熊伟、姜家书、左杰、高琴

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活血消痛酊 挥发性成分 气相色谱-质谱联用法 成分鉴定 含量测定

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(12)