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

摘要/Abstract

摘要：

为了测定养发类化妆品中是否存在激素类和胺类禁用抗菌药物,提出了基于高效液相色谱-串联质谱的养发类化妆品中抗菌药物测定方法。以施华蔻专业修护亮泽活发护理霜为研究对象,使用甲醇作为抗菌药物测定的提取溶液,通过十八烷基硅烷键合硅胶色谱柱,在多反应检测模式下测定养发类化妆品中抗菌药物。结果表明,在施华蔻专业修护亮泽活发护理霜中,10种激素类禁用抗菌药物和3种胺类禁用抗菌药物的检出限均低于定量限,不存在激素类禁用抗菌药物和胺类禁用抗菌药物。激素类抗菌药物的加标回收率和精密度分别为84.7%~114.7%、1.8%~9.8%,胺类禁用抗菌药物的加标回收率和精密度分别为84.1%~93.9%、1.4%~5.7%。分离时长均小于2 min,测定时长均小于4 min,其抗菌药物的测定效率可满足测定需求。

关键词: 高效液相色谱-串联质谱, 养发类化妆品, 抗菌药物, 多反应检测模式

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

中图分类号:

TQ658

何笑薇. 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[J]. 日用化学工业, 2021, 51(8): 789-794.

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.

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参考文献 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