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1.贵州大学 化学与化工学院,贵州 贵阳 550025
2.中国科学院地球化学研究所 环境地球化学 国家重点实验室,贵州 贵阳 550081
余德顺,硕士,研究员,研究方向:生物资源开发与精细化工,E-mail:yudeshun@mail.gyig.ac.cn
收稿日期:2024-09-01,
修回日期:2024-10-12,
录用日期:2024-11-06,
纸质出版日期:2025-05-15
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娄凤华,黄国培,杨军,田弋夫,余德顺.超临界流体色谱-质谱法测定生姜中4种姜酚类物质[J].分析测试学报,2025,44(05):913-918.
LOU Feng-hua,HUANG Guo-pei,YANG Jun,TIAN Yi-fu,YU De-shun.Determination of Four Gingerol Compounds in Ginger by Supercritical Fluid Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(05):913-918.
娄凤华,黄国培,杨军,田弋夫,余德顺.超临界流体色谱-质谱法测定生姜中4种姜酚类物质[J].分析测试学报,2025,44(05):913-918. DOI: 10.12452/j.fxcsxb.240901360.
LOU Feng-hua,HUANG Guo-pei,YANG Jun,TIAN Yi-fu,YU De-shun.Determination of Four Gingerol Compounds in Ginger by Supercritical Fluid Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2025,44(05):913-918. DOI: 10.12452/j.fxcsxb.240901360.
该研究建立了快速测定生姜中6-姜酚、8-姜酚、10-姜酚、6-姜醇的超临界流体色谱-质谱(SFC-MS)方法。使用HSS C
18
SB(100 mm×2.1 mm,1.8 μm)色谱柱,以0.2%(体积分数)甲酸甲醇为改性剂,与超临界流体二氧化碳混合进行梯度洗脱,柱温为40 ℃,背压为13.79 MPa(2 000 psi),进样量为1 μL,流速为1 mL/min,采用电喷雾电离源,正离子选择离子监测模式对目标物定性,外标法定量。结果表明,4种化合物在17 min内完成分析,标准曲线的相关系数(
r
2
)均大于0.995,检出限为0.05~0.08 µg/mL,定量下限为0.5~0.8 µg/mL,平均加标回收率为84.1%~105%,相对标准偏差为0.47%~3.5%,方法具有良好的精密度和准确度。采用SFC-MS法对生姜样品进行分析并与高效液相色谱法进行比较,两者定量结果在误差范围内具有可比性。所建方法的显著优点为分析时间缩短一半,可作为生姜中姜酚类物质的高效快速分析方法。
This study aimed to develop a new method to analyze 6-gingerol,8-gingerol,10-gingerol and 6-shogaol in ginger using supercritical fluid chromatography-mass spectrometry(SFC-MS). Separation was performed using an HSS C
18
SB column(100 mm×2.1 mm,1.8 μm). Gradient elution was employed by the mixture of supercritical carbon dioxide and methanol with 0.2% formic acid as a modifier
. The column temperature was 40 ℃,system back pressure was 13.79 MPa(2 000 psi) ,injection volume was 1 μL,and flow rate was 1 mL/min. Analytes were confirmed and analyzed using electrospray ionization(ESI) in positive ion and selected ion monitoring(SIR) modes,and quantified by external standard method. The results showed that the four target compounds were separated within 17 minutes,the correlation coefficients(
r
²) of the standard curves exceeded 0.995. The detection limits ranged from 0.05 to 0.08 µg/mL,and the quantification limits ranged from 0.5 to 0.8 µg/mL. The average recoveries of standard addition were between 84.1% and 105%,with relative standard deviations between 0.47% and 3.5%. The evaluation indicators demonstrated that the method had good precision and accuracy. The developed method was applied to ginger sample analysis and compared with high performance liquid chromatography(HPLC) method. The quantification results were comparable within the error range. The remarkable advantage of SFC-MS method was that the analysis time was less than half of HPLC method. In conclusion,SFC-MS method can be a novel analysis method for the rapid and efficient analysis of gingerols in ginger.
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