Study of atractylolides determination in Atractylodes lancea (Thunb.) DC.by UPLC-MS/MS

doi:10.16178/j.issn.0528-9017.20231167

Abstract

Abstract:

A method for determination of atractylolide Ⅰ, atractylolide Ⅱ and atractylolide Ⅲ in Atractylodes lancea (Thunb.) DC. by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) was developed and validated. Ion pairs with high ionization effect were obtained via feature scan of mass spectrometry. The samples were extracted with methanol at room temperature, the liquid-solid ratio was 20 mL·g^-1, and the ultrasonic extraction time was 45 min. The extraction amount of the three atractylolides reached a high level, which were 621.33、201.32 and 275.97 μg·g^-1 respectively; The recoveries of the three atractylodes were in the range of 85.7%-106.2% with the relative standard deviations of 6.0%-9.7%. The detection limit and quantification limit of the method are 18.2-32.2 μg·L^-1 and 61.0-111.2 μg·L^-1, respectively. This method can be suitable for the simultaneous analysis of three atractylodes in Atractylodes lancea.

Key words: UPLC-MS/MS, Atractylodes lancea (Thunb.) DC., atractylolides

CLC Number:

S567.23

ZHANG Wenwen, WU Qinyan, ZHAO Laicheng, LIANG Hongfang, WANG Jianhua, CHEN Lu. Study of atractylolides determination in Atractylodes lancea (Thunb.) DC.by UPLC-MS/MS[J]. Journal of Zhejiang Agricultural Sciences, 2025, 66(4): 923-927.

Figures/Tables 6

References 14

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化合物	分子量/ (g·mol^-1)	母离子 (m/z)	子离子 (m/z)	去簇电压/V	碰撞能/V
苍术内酯Ⅰ	230.3	231.3	188.2^*,158.2	120	25,30
苍术内酯Ⅱ	232.3	233.2	188.2^*,216.1	100	23,30
苍术内酯Ⅲ	248.3	266.3	250.2^*,232.1	40	8,20

化合物	分子量/ (g·mol^-1)	母离子 (m/z)	子离子 (m/z)	去簇电压/V	碰撞能/V
苍术内酯Ⅰ	230.3	231.3	188.2^*,158.2	120	25,30
苍术内酯Ⅱ	232.3	233.2	188.2^*,216.1	100	23,30
苍术内酯Ⅲ	248.3	266.3	250.2^*,232.1	40	8,20

化合物	线性范围/(μg·L^-1)	标准曲线方程	相关系数(R²)	检测限/(μg·L^-1)	定量限/(μg·L^-1)
苍术内酯I	31.25~500	y=1 066.72x+1 665.183 4	0.998 96	18.2	61.0
苍术内酯Ⅱ	31.25~500	y=2 548.40x-1 904.799 50	0.999 75	19.5	64.5
苍术内酯Ⅲ	31.25~500	y=282.875 8x+98.613 84	0.998 83	32.2	111.2

化合物	线性范围/(μg·L^-1)	标准曲线方程	相关系数(R²)	检测限/(μg·L^-1)	定量限/(μg·L^-1)
苍术内酯I	31.25~500	y=1 066.72x+1 665.183 4	0.998 96	18.2	61.0
苍术内酯Ⅱ	31.25~500	y=2 548.40x-1 904.799 50	0.999 75	19.5	64.5
苍术内酯Ⅲ	31.25~500	y=282.875 8x+98.613 84	0.998 83	32.2	111.2

化合物	加标量/ (μg·g^-1)	回收率/%	相对标准偏差/%
苍术内酯Ⅰ	320、160、80	88.1、91.7、102.3	6.0、9.7、9.4
苍术内酯Ⅱ	160、80、40	104.2、106.2、85.7	6.8、6.7、9.5
苍术内酯Ⅲ	160、80、40	101.7、86.1、95.7	7.7、9.6、9.1