高效液相色谱-串联质谱法快速测定养发类化妆品中抗菌药物

doi:10.3969/j.issn.1001-1803.2021.08.014

Abstract

Abstract:

In order to determine the hormone- and amine-type forbidden antibacterial drugs in hair-care cosmetics, a high performance liquid chromatography-tandem mass spectrometry-based method for was proposed. Taking Schwarzkopf professional repairing and brightening hair care cream as the research object, using methanol as the extraction solution, the antibacterial drugs in hair care cosmetics were determined by octadecylsilane-bonded silica gel chromatographic column in multi-reaction detection mode. The results show that when 0.02 mol/L ammonium formate aqueous solution is used as the flow phase, the superimposed total ion current separation effect of hormone-type forbidden antibacterial drugs in hair care cosmetics is the best. The isotope abundance ratio is the highest. When the extraction solvent is methanol, the recovery rates of A-1 to A-10 hormone-type and B-1, B-2, and B-3 amine-type forbidden antibacterial drugs are the highest, which are greater than 90% and 95%, respectively. For this reason, this article uses methanol as the sample extraction solution for the determination of 10 hormone-type forbidden antibacterial drugs. The results show that in Schwarzkopf Professional Repairing and Brightening Hair Care Cream, the detection limits of 10 hormone-type forbidden antibacterial drugs and 3 amine-type forbidden antibacterial drugs are all lower than the quantitative limit. The recovery and precision of hormone-type forbidden antibacterial drugs are 84.7%-114.7% and 1.8%-9.8%, respectively. The recovery and precision of amine-type forbidden antibacterial drugs are 84.1%-93.9% and 1.4%-5.7%, respectively. The separation time is less than 2 min and the determination time is less than 4 min. In Schwarzkopf Professional Repairing and Brightening Hair Care Cream, there are no hormone-type forbidden antibacterial drugs and amine-type forbidden antibacterial drugs, and the measurement efficiency of antibacterial drugs can meet the measurement requirements.

Key words: high performance liquid chromatography-tandem mass spectrometry, hair care cosmetics, antimicrobial agents, multi-reaction detection mode

CLC Number:

TQ658

He Xiaowei. Rapid determination of antimicrobial agents in hair care cosmetics by high performance liquid chromatography-tandem mass spectrometry[J].China Surfactant Detergent & Cosmetics, 2021, 51(8): 789-794.

Figures/Tables 11

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References 14

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编码	抗菌药物类型	前体离子（m/z）	子离子（m/z）	碰撞能量/eV
A-1	米诺地尔	210.1	164.2^*,193.3	26,11
A-2	螺内酯	341.2	107.2^*, 90.8	36,66
A-3	雌酮	271.3	253.2^*,132.9	6,23
A-4	坎利酮	341.2	107.2^*, 90.8	36,66
A-5	黄体酮	315.3	97.1^*,109.1	24,24
A-6	可的松	361.2	163.2^*,121.1	21,31
A-7	氢化可的松	363.2	121.1^*,327.1	11,26
A-8	氟米松	411.2	253.1^*,121.2	11,35
A-9	氟米龙	377.3	278.8^*,320.8	11, 9
A-10	曲安奈德醋酸酯	477.4	457.3^*,439.2	5,11

编码	抗菌药物类型	前体离子（m/z）	子离子（m/z）	碰撞能量/eV
B-1	氟他胺	277.2	161.2^*,231.2	26,21
B-2	度他雄胺	529.5	461.4^*, 95.2	46,35
B-3	非那雄胺	373.4	305.4^*,317.4	31,23

抗菌药物类型	回收率/%
抗菌药物类型	20%氯化钠-乙腈	甲醇	乙腈
A-1	89.2	91.2	89.1
A-2	89.3	92.1	88.3
A-3	89.1	90.3	88.9
A-4	88.3	90.4	88.3
A-5	88.9	90.2	89.1
A-6	88.3	90.2	88.3
A-7	89.4	90.3	88.9
A-8	89.2	90.4	88.3
A-9	89.3	91.3	88.3
A-10	88.2	94.2	88.1

抗菌药物类型	线性方程	相关系数	回收率、精密度/%		检出限/（μg·kg^-1）	定量限/（μg·kg^-1）
抗菌药物类型	线性方程	相关系数	水平a	水平b	检出限/（μg·kg^-1）	定量限/（μg·kg^-1）
A-1	y=11 598.2x-2 402.8	0.999 9	91.8（1.8）	100.9（2.4）	2	4
A-2	y=315.9x+830.2	0.999 4	86.5（5.3）	106.4（2.5）	21	61
A-3	y=1 968.7x-2 462.5	0.999 8	84.7（3.7）	97.2（2.0）	11	31
A-4	y=3 736.9x+1 527.3	0.999 8	94.9（3.6）	109.2（1.9）	6	16
A-5	y=649.8x-392.2	0.999 8	89.1（4.3）	101.7（2.6）	11	31
A-6	y=503.7x+1 597.2	0.999 5	94.2（3.6）	110.8（3.3）	11	31
A-7	y=384.4x+6 784.2	0.999 9	86.3（9.8）	114.7（2.5）	11	31
A-8	y=397.3x+2 459.9	0.999 2	92.6（8.3）	114.7（3.9）	11	31
A-9	y=1 266.9x+5 612.3	0.999 1	90.6（5.9）	111.3（1.8）	6	16
A-10	y=2 204.5x+2 125.9	0.999 8	101.8（7.2）	114.7（2.7）	11	31

抗菌药物类型	线性方程	相关系数	检出限/（μg·kg^-1）	定量限/（μg·kg^-1）
B-1	y=48.9x+16.6	0.999 1	13.4	40.1
B-2	y=448.1x+87.9	0.998 9	1.8	5.1
B-3	y=445.1x-141.3	0.998 9	1.4	4.1

Rapid determination of antimicrobial agents in hair care cosmetics by high performance liquid chromatography-tandem mass spectrometry

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提取溶剂	回收率/%
提取溶剂	B-1	B-2	B-3
乙酸乙酯	90	80	85
乙腈	90	85	84
丙酮	90	90	90
甲醇	91	95	95

抗菌药物类型	回收率、精密度/%
抗菌药物类型	加标水平a	加标水平b	加标水平c
B-1	86.3（5.7）	88.1（3.1）	92.1（2.8）
B-2	84.1（4.1）	89.8（2.0）	93.9（1.4）
B-3	86.2（4.0）	91.6（3.6）	92.2（2.1）

抗菌药物类型	分离时长/min	测定时长/min	是否满足测定需求
A-1	1.21	3.87	是
A-2	1.09	3.23	是
A-3	1.11	3.24	是
A-4	1.21	3.22	是
A-5	1.08	3.23	是
A-6	1.23	3.21	是
A-7	1.21	3.23	是
A-8	1.23	3.22	是
A-9	1.21	3.21	是
A-10	1.23	3.19	是

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