高效液相色谱-串联质谱法测定美白类化妆品中5种荧光增白剂

doi:10.3969/j.issn.1001-1803.2020.06.012

Abstract

Abstract:

A method for the determination of five fluorescent whitening agents （FWAs） in cosmetics by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was developed. The samples were extracted with 50% methanol by ultrasonic extraction for 30 min, purified by WAX SPE column, and analyzed by HPLC-MS/MS on a CAPCELL PAK-C₁₈ column （2.0 mm×150 mm, 3 μm）, employing methanol-5 mmol/L ammonium acetate as mobile phase in a gradient elution mode. Electrospray ionization （ESI） source was operated in the negative mode using multiple reaction monitoring （MRM） scanning mode. The results were quantified by external standard method. The results indicated that the method had good linear relationships with correlation coefficients （r） greater than 0.99. The limits of detection（LODs） are 0.1-1.01 mg/L and the limits of quantification （LOQs） are 0.33-2.03 mg/L. The average recoveries at three spiked levels are in the range of 90.6%-113.2%, and the relative standard deviations （RSDs） are in the range of 2.2%-14.1%.

Key words: HPLC-MS/MS, fluorescent whitening agents, solid phase extraction, cosmetics

CLC Number:

TQ658

DOU Yue,TIAN Jin-qiang,WANG Qian-lei,WANG Yong-feng,PAN Ke-yi. Determination of five fluorescent whitening agents in cosmetics by high performance liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2020, 50(6): 427-432.

Figures/Tables 6

Fig. 1

Tab. 1

Fig. 2

Tab. 2

Tab. 3

Tab. 4

References 15

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化合物	化学文摘号	母离子（m/z）	子离子（m/z）	锥孔电压/eV	碰撞能/eV
FWA220	4193-55-9	537.3	309.2*	-90	-45
FWA220	4193-55-9	537.3	197	-90	-60
FWA357	41098-56-0	585.5	545.6*	-85	-35
FWA357	41098-56-0	585.5	505.4	-85	-40
FWA85	12224-06-5	827.3	623*	-130	-60
FWA85	12224-06-5	827.3	543.4	-130	-75
FWA113	12768-92-2	915.2	587.3*	-145	-85
FWA113	12768-92-2	915.2	667.1	-145	-70
FWA71	16090-02-1	879.2	569.3*	-150	-80
FWA71	16090-02-1	879.2	649.2	-150	-70

化合物	回收率/%
化合物	WAX	HLB	NH₂	MAX	CN
FWA85	83.3	56.3	75.9	0	0
FWA220	101.1	65.3	86.0	0	0
FWA357	86.7	77.0	94.7	0	0
FWA71	102.3	65.6	66.3	0	0
FWA113	102.4	63.7	63.2	0	0

剂型	化合物	线性范围/（mg·L^-1）	线性方程	相关系数	检出限/（mg·L^-1）	定量限/（mg·L^-1）
水剂	FWA220	0.10~10.20	y = 1 180x-298	0.998 6	0.14	0.49
	FWA357	0.11~11.15	y = 407x-308	0.992 7	1.01	2.03
	FWA85	0.12~12.26	y = 958x+31	0.997 4	0.10	0.36
	FWA113	0.12~12.18	y = 1 160x-577	0.997 5	0.10	0.35
	FWA71	0.10~10.44	y = 1 310x-192	0.993 4	0.10	0.33
乳剂	FWA220	0.10~10.20	y = 882x-128	0.998 9	0.14	0.49
	FWA357	0.11~11.15	y = 286x-174	0.997 8	1.01	2.03
	FWA85	0.12~12.26	y = 443x+129	0.998 2	0.10	0.36
	FWA113	0.12~12.18	y = 778x+50	0.997 3	0.10	0.35
	FWA71	0.10~10.44	y = 684x-274	0.997 1	0.10	0.33
清洁剂	FWA220	0.10~10.20	y = 1 090x-446	0.996 9	0.14	0.49
	FWA357	0.11~11.15	y = 355x-255	0.994 6	1.01	2.03
	FWA85	0.12~12.26	y = 701x-139	0.998 8	0.10	0.36
	FWA113	0.12~12.18	y = 832x-455	0.996 6	0.10	0.35
	FWA71	0.10~10.44	y = 840x-18.1	0.999 5	0.10	0.33

化合物	加入量/（mg·L^-1）	水剂		乳剂		清洁剂
化合物	加入量/（mg·L^-1）	平均回收率/%	相对标准偏差/%	平均回收率/%	相对标准偏差/%	平均回收率/%	相对标准偏差/%
FWA85	1	96.9	11.6	90.6	6.6	98.4	6.8
	5	96.3	9.5	102.7	7.7	101.2	5.0
	10	102.2	7.3	107.5	2.2	96.6	3.0
FWA220	1	96.4	8.0	98.8	6.5	102.3	4.8
	5	94.1	5.0	91.5	5.4	93.1	5.7
	10	104.2	3.3	103.4	4.1	92.1	3.6
FWA357	1	93.8	13.5	101.9	7.4	99.8	9.7
	5	92.9	5.8	94.7	7.1	86.8	9.1
	10	111.6	6.5	103.0	3.6	93.0	6.4
FWA71	1	108.2	8.2	97.6	14.1	111.9	10.0
	5	100.4	9.5	102.1	10.1	111.3	13.1
	10	97.3	6.2	98.9	8.5	113.2	8.0
FWA113	1	95.4	10.4	98.0	12.5	105.1	10.2
	5	92.1	7.2	93.2	6.0	94.0	8.7
	10	97.7	4.6	92.7	4.3	110.1	7.9

Determination of five fluorescent whitening agents in cosmetics by high performance liquid chromatography-tandem mass spectrometry

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