LC-MS/MS法测定蜂胶类牙膏中白杨黄素的含量

doi:10.3969/j.issn.1001-1803.2019.01.012

Abstract

Abstract:

The chrysin （ChR） in propolis toothpaste was extracted by methanol, purified by freezing centrifugation, separated by Diamonsil C₁₈ column （4.6 mm×250 mm, 5 μm） and detected by mass spectrometry. A liquid chromatography-tandem mass spectrometry （LC-MS/MS） method was established to determine the content of ChR in propolis toothpaste. The results show that ChR has a good linear relationship in the range of 5.0-100.0 μg/L mass concentration, and the correlation coefficients （R ²） was 0.999 8. The detection limit is 1.5 μg/kg and the limit of quantification is 5.0 μg/kg. The average recovery of the spiked standard is 93.0% to 100.1%, and the relative standard deviation （RSD） is 1.3% to 3.4%.

Key words: propolis toothpaste, chrysin, propolis extract, liquid chromatography-tandem mass spectrometry

CLC Number:

TQ658.4

Ya-nan HAN,Hui-feng SU. Determination of the content of chrysin in propolis toothpaste by LC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2019, 49(1): 58-62.

Figures/Tables 5

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Tab. 2

References 16

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样品	加标量/（μg·kg^-1）	实测值/（μg·kg^-1）						平均回收率/%	RSD/%
样品	加标量/（μg·kg^-1）	1	2	3	4	5	6	平均回收率/%	RSD/%
牙膏1	5.0	4.84	4.66	4.91	4.94	4.94	4.91	97.3	2.1
	50.0	4.86	4.99	4.89	5.09	4.94	4.94	99.0	1.7
	100.0	4.89	4.84	4.81	4.94	4.95	4.98	98.0	1.9
牙膏2	5.0	4.94	4.94	4.89	4.94	4.82	4.86	97.9	1.5
	50.0	4.47	4.91	4.57	4.94	4.86	4.92	95.5	1.9
	100.0	4.94	4.99	5.03	4.94	5.15	4.99	100.1	2.8
牙膏3	5.0	4.94	4.91	4.79	4.79	4.95	4.79	97.2	1.3
	50.0	4.79	4.48	4.94	4.94	4.44	4.91	94.9	1.7
	100.0	4.69	4.89	4.78	4.34	4.76	4.47	93.0	3.4

检测方法	线性范围/（mg·L^-1）	回收率/%	RSD/%	检出限	定量限	参考文献
HPLC	5.0~200.0	95.5~100.8	1.1~2.0	0.4 mg/L	1.4 mg/L	[1]
HPLC	5.0~80.00	100.9	0.9	0.04 mg/L	0.1 mg/L	[9]
LC-MS	0.004~4.00000	90.0~96.3	4.6~6.2	1.5 μg/L	4.0 μg/L	[13]
HPLC	0.5~200.0	92.6~101.4	2.1~3.6	0.1 μg/kg	0.5 mg/kg	QB/T 5289-2018
LC-MS/MS	0.005~0.10000	93.0~100.1	1.3~3.4	1.5 μg/kg	5.0 μg/kg	本方法

Determination of the content of chrysin in propolis toothpaste by LC-MS/MS

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