高效液相色谱法测定化妆品中香豆素类化合物

doi:10.3969/j.issn.1001-1803.2020.03.012

摘要/Abstract

摘要：

建立了化妆品中8-羟基补骨脂素、补骨脂素、异补骨脂素、8-甲氧基补骨脂素、5-甲氧基补骨脂素、三甲沙林、欧前胡素、异欧前胡素8种香豆素类化合物含量鉴定的高效液相色谱分析方法。样品经超临界CO₂萃取法提取,其中以甲醇作为载体助溶剂。采用Agilent ZORBAX Eclipse Plus C₁₈色谱柱（250 mm×4.6 mm×5 μm）作为分析柱,乙腈和水作为二元流动相,柱温25 ℃,流速1.0 mL/min,检测波长250 nm,外标法定量。结果表明,8种化合物的线性相关系数均大于0.999,低、中、高3种加标水平下的平均加标回收率为85.1%~110.0%,相对标准偏差RSD<6.42% （n=6）。该方法简单、高效、准确,为化妆品中香豆素类化合物定量提供了一种有效的分析技术。

关键词: 化妆品, 香豆素类化合物, 高效液相色谱, 超临界CO₂萃取

Abstract:

A high performance liquid chromatographic （HPLC） method was developed for the simultaneous determination of 8 coumarin compounds in cosmetics, including 8-hydroxypsoralen, psoralen, isopsoralen, 8-methoxypsoralen, 5-methoxypsoralen, trioxsalen, imperatorin and isoimperatorin. The samples were extracted by supercritical CO₂ extraction with methanol as carrier cosolvent. Chromatographic separation was achieved on an Agilent ZORBAX Eclipse Plus C₁₈ chromatographic column （250 mm×4.6 mm×5 μm, column temperature 25 ℃） through gradient elution with acetonitrile-water as binary mobile phase at a flow rate of 1.0 mL/min, and the detection wavelength was 250 nm. The external standard method was used for quantification. The results showed that the linear correlation coefficients of the 8 compounds were all greater than 0.999; the average recoveries at three spiked levels were in the range of 85.1%-110.0% with RSDs （n=6） lower than 6.42%. This method was proved to be simple, efficient and accurate, which provided an effective detection technique for coumarin compounds in cosmetics.

Key words: cosmetics, coumarin compounds, high performance liquid chromatography, supercritical CO₂ extraction

中图分类号:

TQ658

刘国清,李静,许建帼,吕延文,潘向军,董云渊. 高效液相色谱法测定化妆品中香豆素类化合物[J]. 日用化学工业, 2020, 50(3): 204-207.

Guo-qing LIU,Jing LI,Jian-guo XU,Yan-wen LV,Xiang-jun PAN,Yun-yuan DONG. Determination of coumarins in cosmetics by high performance liquid chromatography[J]. China Surfactant Detergent & Cosmetics, 2020, 50(3): 204-207.

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参考文献 19

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名称	CAS	保留时间/min	线性范围/（mg·L^-1）	线性方程	相关系数	检出限/（mg·kg^-1）	定量限/（mg·kg^-1）
8-羟基补骨脂素	2009-24-7	6.269	0.01~5	y=47 442.3x-2.261 46	0.999 9	0.3	1
补骨脂素	66-97-7	10.214	0.01~5	y=67 352.1x-5 825.40	0.999 7	0.3	1
异补骨脂素	523-50-2	10.738	0.01~5	y=70 906.2x+382.449	0.999 9	0.3	1
8-甲氧基补骨脂素	298-81-7	11.545	0.01~5	y=61 090.0x+48.686 8	0.999 9	0.3	1
5-甲氧基补骨脂素	484-20-8	14.641	0.01~5	y=45 116.7x+52.289 2	0.999 9	0.3	1
三甲沙林	3902-71-4	19.778	0.01~5	y=80 737.8x+437.453	0.999 9	0.3	1
欧前胡素	482-44-0	20.297	0.01~5	y=49 736.0x+188.207	0.999 9	0.3	1
异欧前胡素	482-45-1	22.830	0.01~5	y=42 247.4x+377.626	0.999 9	0.3	1

名称	平均加标回收率/%			相对标准偏差RSD/%
名称	低水平	中水平	高水平	低水平	中水平	高水平
8-羟基补骨脂素	100.3	110.0	105.0	1.89	1.82	2.82
补骨脂素	87.5	103.0	100.9	1.96	1.86	1.98
异补骨脂素	98.4	104.3	102.8	1.95	1.89	2.08
8-甲氧基补骨脂素	91.8	104.2	102.0	0.78	1.79	2.10
5-甲氧基补骨脂素	94.4	102.5	107.7	6.24	1.85	0.76
三甲沙林	96.3	102.7	101.7	2.48	1.75	1.88
欧前胡素	86.9	101.1	100.4	6.42	1.50	1.72
异欧前胡素	85.1	97.8	99.7	2.58	2.34	1.92

前处理方法	前处理时间/min	提取溶剂用量（以1 g样品为基准）	加标回收率/%	文献
甲醇超声提取	≥30	≥10 mL甲醇	86.0~106.3	[ 8 ]
甲醇超声提取	≥30	≥10 mL甲醇	90.5~106.4	[ 9 ]
甲醇/乙醇超声提取	≥30	≥10 mL甲醇/乙醇	85.0~105.8	[12]
超临界二氧化碳（CO₂）萃取	20	0.2 g甲醇	85.1~110.0	本文