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

摘要/Abstract

摘要：

采用甲醇提取蜂胶类牙膏中白杨黄素（ChR） ,冷冻离心净化,经Diamonsil C₁₈ （4.6 mm×250 mm,5 μm）色谱柱分离,质谱检测器检测,建立了液相色谱-串联质谱法（LC-MS/MS）测定蜂胶类牙膏中ChR含量。结果表明,ChR在5.0~ 100.0 μg/L质量浓度范围内呈现良好的线性关系,相关系数（R ²）为0.999 8;检出限为1.5 μg/kg,定量限为5.0 μg/kg;加标回收率为93.0%~100.1%,相对标准偏差（RSD）为1.3%~3.4%。

关键词: 蜂胶类牙膏, 白杨黄素, 蜂胶提取物, 液相色谱-串联质谱法

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

中图分类号:

TQ658.4

韩雅楠,苏慧锋. LC-MS/MS法测定蜂胶类牙膏中白杨黄素的含量[J]. 日用化学工业, 2019, 49(1): 58-62.

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.

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参考文献 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