高效液相色谱法同时测定淋洗类化妆品中7种异噻唑啉酮类防腐剂及质谱确证

doi:10.3969/j.issn.2097-2806.2024.10.015

Abstract

Abstract:

An analytical method for the simultaneous determination of seven isothiazolinone preservatives in rinse-off cosmetics by high-performance liquid chromatography （HPLC） and verification by liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was established. The cream and liquid cosmetic samples were ultrasonically extracted with methanol, centrifuged, and the supernatant was filtered through a microporous membrane for determination. The separation was executed on a CAPCELL PAK C₁₈ MGIII column by gradient elution at a flow rate of 1.0 mL/min with methanol and 0.1% （V/V） phosphoric acid aqueous solution as the mobile phases. The column temperature was set at 40 ℃. The wavelengths of detection were 278, 282 and 319 nm. The results of high performance liquid chromatography were used for qualitative screening, the standard curve method was used for quantification, and the results of liquid chromatography tandem mass spectrometry were used for verification. The results show that the linear ranges of the seven isothiazolinone preservatives are 0.1-50 mg/L, and the correlation coefficients are all greater than 0.999 9. The average recoveries are 97.5%-109.9% （for cream） and 95.6%-103.6% （for liquid）, and the relative standard deviations （RSD） are bellow 3.0% at low, medium and high spiked levels. The detection limits are 0.05-0.11 mg/kg. The method is simple, rapid and accurate for the simultaneous determination and verification of seven isothiazolinone preservatives in the rinse-off cosmetics.

Key words: rinse-off cosmetics, high performance liquid chromatography, mass spectrometric verification, isothiazolinone preservatives

CLC Number:

TQ658

Cen Chen, Beizhou Cui, Liyuan Zhang, Linqi Yan, Qiaoyuan Cheng. Simultaneous determination of seven isothiazolinone preservatives in rinse-off cosmetics by HPLC and verification by HPLC-MS/MS[J].China Surfactant Detergent & Cosmetics, 2024, 54(10): 1268-1275.

Figures/Tables 9

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References 20

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序号	化合物	母离子（m/z）	子离子（m/z）	CE/eV	相对离子丰度/%	允许相对偏差/%
1	MIT	116.0	100.8^*，84.9	31, 33	100, 50	25
2	CMIT	150.0	87.0^*，115.0	51, 29	100, 22	25
3	BIT	152.0	134.1^*，77.1	39, 33	100, 23	25
4	MBIT	166.0	151.0^*，96.0	33, 48	100, 65	20
5	BBIT	208.0	151.9^*，108.9	24, 34	100, 37	25
6	OIT	214.1	102.1^*，57.2	21, 22	100, 53	20
7	DCOIT	282.0	170.0^*，71.0	23, 26	100, 32	25

化合物	保留时间/min	线性范围/（mg/L）	回归方程	相关系数r	LOD/（mg/kg）	LOQ/（mg/kg）
MIT	3.20	0.1~50	Y=44 505X+3 104	0.999 9	0.05	0.18
CMIT	5.17	0.1~50	Y=27 280X+1 562	1.000 0	0.09	0.31
BIT	6.43	0.1~50	Y=22 017X+661	1.000 0	0.11	0.37
MBIT	7.07	0.1~50	Y=20 914X+800	1.000 0	0.10	0.32
BBIT	9.53	0.1~50	Y=15 594X+976	1.000 0	0.08	0.39
OIT	10.20	0.1~50	Y=23 071X+1 663	0.999 9	0.09	0.27
DCOIT	12.72	0.1~50	Y=19 385X+851	1.000 0	0.08	0.26

化合物	加标浓度水平/（mg/kg）	平均回收率/%		RSD/%
化合物	加标浓度水平/（mg/kg）	膏霜乳	液体	膏霜乳	液体
MIT	5	105.6	99.8	2.50	0.62
	50	104.1	100.2	0.98	0.69
	400	98.6	95.7	1.67	1.42
CMIT	5	105.9	96.6	1.45	1.60
	50	104.3	101.0	0.98	0.86
	400	102.9	99.6	1.67	1.41
BIT	5	109.9	97.6	1.07	1.61
	50	104.1	102.2	0.96	0.70
	400	98.4	95.8	0.97	0.38
MBIT	5	105.7	103.6	2.02	1.95
	50	103.7	102.4	0.92	0.76
	400	97.5	95.6	0.75	0.77
BBIT	5	101.8	97.7	1.73	1.84
	50	105.7	102.1	0.94	0.76
	400	102.7	99.6	1.67	1.38
OIT	5	98.6	95.7	1.64	2.52
	50	102.9	102.5	0.92	0.67
	400	98.8	97.6	0.36	0.71
DCOIT	5	104.1	99.8	1.02	1.83
	50	104.5	101.1	0.99	0.79
	400	101.9	100.3	0.50	0.35

化合物	检出限/ ng	定量限/ ng	检出浓度/（mg/kg）	定量浓度/（mg/kg）
MIT	1.02	3.42	0.001 0	0.003 4
CMIT	1.08	3.61	0.001 1	0.003 6
BIT	1.88	6.25	0.001 9	0.006 3
MBIT	0.51	1.72	0.000 51	0.001 7
BBIT	0.35	1.17	0.000 35	0.001 2
OIT	0.28	0.93	0.000 28	0.000 9
DCOIT	1.64	5.47	0.001 6	0.005 5

Simultaneous determination of seven isothiazolinone preservatives in rinse-off cosmetics by HPLC and verification by HPLC-MS/MS

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