超高效液相色谱-三重四极杆/线性离子阱串联质谱法测定睫毛相关化妆品中的7种前列腺素类似物

doi:10.3969/j.issn.2097-2806.2025.06.016

Abstract

Abstract:

A method based on ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry （UPLC-QTRAP-MS/MS） has been developed for the detection and quantification of 7 prostaglandin analogs in eyelash-related cosmetics. Samples were extracted with methanol via ultrasonic extraction and separated on an ACE Excel 2 C₁₈ （100 mm× 2.1 mm, 2 μm） column using a mobile phase of acetonitrile-5 mmol/L ammonium acetate （containing 0.05% formic acid） in a gradient elution mode. Data were collected in the ESI⁺ mode using multiple reaction monitoring （MRM） combined with enhanced product ion scanning （EPI）. Quantification was performed using matrix-matched external standard calibration curves, with both retention times and the ratios of ion pair abundances serving as the basis for qualitative assessments. Further confirmation of target components was achieved through comparison of EPI spectra. The results reveal a strong linear correlation for the 7 prostaglandin analogs within their respective linearity ranges, with the correlation coefficients exceeding 0.999. Sensitivity is characterized by the detection limits ranging from 0.002 0 to 0.020 μg/g and quantitation limits from 0.005 0 to 0.050 μg/g. The average recoveries at three spiked levels are found to be between 87.3% and 107.0%, with the RSDs varying from 0.7% to 5.4% （n=6）. This method is used to analyze 9 batches of eyelash-related cosmetics, and 1 batch is found to contain bimatoprost. The developed method, distinguished by its operational straightforwardness, analytical precision, and detection sensitivity, is adeptly applicable for the quantitative determination and qualitative screening of the 7 prostaglandin analogs in cosmetics.

Key words: ultra-high performance liquid chromatography-triple quadrupole/linear ion trap mass spectrometry, enhanced product ion scan, prostaglandin analogs, eyelash enhancing, cosmetics

CLC Number:

TQ658

Xu Gong, Jing Sun, Youlong Feng. Determination of 7 prostaglandin analogsin eyelash-related cosmetics by UPLC-QTRAP-MS/MS[J].China Surfactant Detergent & Cosmetics, 2025, 55(6): 811-816.

Figures/Tables 7

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References 15

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编号	化合物名称	保留时间/min	母离子（m/z）	子离子（m/z）	碰撞电压/V	锥孔电压/V
1	比马前列素	4.13	398.3	362.3^*, 317.2	12, 20	70
2	他氟乙酰胺	4.95	438.3	306.2^*, 288.3	14, 18	60
3	乌诺前列酮	6.05	383.2	329.1^*, 205.1	17, 23	80
4	拉坦前列素	6.37	433.3	397.3^*, 337.2	14, 20	80
5	曲伏前列素	6.56	501.2	321.2^*, 303.0	10, 8	80
6	他氟前列素	7.08	453.3	335.1^*, 261.2	10, 8	60
7	乌诺前列酮异丙酯	8.48	425.2	329.2^*, 247.1	20, 22	80

序号	化合物名称	线性回归方程		线性范围/（ng/mL）	r	LOD/（μg/g）	LOQ/（μg/g）
序号	化合物名称	精华液	凝胶	线性范围/（ng/mL）	r	LOD/（μg/g）	LOQ/（μg/g）
1	比马前列素	y=219 030x+5 243.11	y=231 499x+5 921.35	0.099 4~49.7	0.999 8	0.002 0	0.005 0
2	他氟乙酰胺	y=183 793x+3 791.75	y=189 917x+3 969.94	0.099 9~50.0	0.999 9	0.002 0	0.005 0
3	乌诺前列酮	y=78 600.5x-4.783 05	y=75 742.6x+403.267	1.00~500	0.999 8	0.020	0.050
4	拉坦前列素	y=134 250x+1 808.95	y=134 322x+1 342.75	0.099 4~49.7	0.999 9	0.002 0	0.005 0
5	曲伏前列素	y=103 376x+4 214.69	y=104 722x+2 587.49	0.199~99.6	0.999 4	0.004 0	0.010
6	他氟前列素	y=125 428x+1 484.44	y=119 479x+536 037	1.00~500	0.999 9	0.020	0.050
7	乌诺前列酮异丙酯	y=50 354.5x+2 027.88	y=45 434.2x+615.005	0.040 0~50.0	0.999 7	0.002 0	0.005 0

序号	化合物	添加水平/（μg/g）	精华液		凝胶
序号	化合物	添加水平/（μg/g）	平均回收率/%	RSD/%	平均回收率/%	RSD/%
1	比马前列素	0.009 9	98.4	2.9	96.1	1.1
		0.25	103.6	0.8	103.9	2.0
		0.99	101.5	1.5	100.8	3.6
2	他氟乙酰胺	0.010	99.2	2.6	101.0	2.2
		0.25	103.0	1.7	106.3	0.9
		1.0	100.0	0.8	102.3	1.4
3	乌诺前列酮	0.10	99.5	4.0	100.0	2.7
		2.5	95.2	2.3	99.8	1.1
		10	96.1	1.3	97.1	1.6
4	拉坦前列素	0.009 9	102.9	4.2	101.8	4.1
		0.25	100.9	3.2	102.5	2.8
		0.99	98.3	1.2	98.2	2.1
5	曲伏前列素	0.020	87.3	5.4	93.5	4.4
		0.50	100.3	2.0	107.0	3.1
		2.0	101.6	3.0	102.6	2.3
6	他氟前列素	0.10	101.0	4.5	96.2	3.9
		2.5	99.3	1.3	106.7	1.2
		10	96.9	0.7	98.4	1.2
7	乌诺前列酮异丙酯	0.010	88.8	5.0	96.7	3.7
		0.25	99.3	1.5	101.9	0.9
		1.0	96.8	1.0	98.9	1.1

序号	化合物名称	基质效应
序号	化合物名称	精华液	凝胶	乳液
1	比马前列素	0.99	1.10	1.10
2	他氟乙酰胺	0.98	1.00	1.00
3	乌诺前列酮	0.97	0.94	0.90
4	拉坦前列素	1.00	1.00	0.96
5	曲伏前列素	0.88	0.89	0.88
6	他氟前列素	0.98	0.93	0.88
7	乌诺前列酮异丙酯	0.99	0.89	0.84

Determination of 7 prostaglandin analogsin eyelash-related cosmetics by UPLC-QTRAP-MS/MS

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