HPLC-MS/MS法测定洗发水中10种违禁药物

doi:10.3969/j.issn.1001-1803.2020.03.011

摘要/Abstract

摘要：

采用甲醇稀释和高效液相色谱-串联质谱仪,建立了洗发水中10种违禁药物的检测方法。样品经甲醇超声萃取后,以0.1% （v/v）甲酸水溶液和乙腈为流动相,C18色谱柱梯度洗脱分离,采用电喷雾正、负离子源同时采集,多反应监测（MRM）模式进行检测。结果表明,该方法10种化合物在0.2 ~ 10 μg/L内均有良好的线性,相关系数大于0.99;添加浓度水平为10~50 μg/kg时,平均回收率为90.5% ~ 94.2%,相对标准偏差（RSD）为2.3% ~ 4.8%,方法检出限为0.8 ~ 2.4 μg/kg,定量限为2.6 ~7.9 μg/kg。

关键词: 洗发水, 高效液相色谱-串联质谱法, 违禁药物, 检测

Abstract:

A method for the determination of 10 prohibited drugs in shampoo by high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） was established. The samples were ultrasonic extracted with methanol, separated on a C18 columm by gradient elution with 0.1% （v/v） formic acid solution and acetonitrile as mobile phases, and finally analyzed using electrospray ionization in positive and negative ion mode with multiple reaction monitoring （MRM）. The linear ranges of the 10 compounds were from 0.2 to 10 μg /L with the correlation coefficients （r ²） more than 0.99. The average recoveries and relative standard deviations were 90.5%-94.2% and 2.3%-4.8% respectively in the spiked ranges of 10-50 μg/kg. The limit of detection and quantification were 0.8-2.4 μg/kg and 2.6-7.9 μg/kg, respectively.

Key words: shampoo, HPLC-MS/MS, prohibited drugs, detection

中图分类号:

TQ658.3

杨旺火. HPLC-MS/MS法测定洗发水中10种违禁药物[J]. 日用化学工业, 2020, 50(3): 199-203.

Wang-huo YANG. Determination of 10 prohibited drugs in shampoo by high performance liquid chromatography-tandem mass spectrometry[J]. China Surfactant Detergent & Cosmetics, 2020, 50(3): 199-203.

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化合物	电离模式	母离子（m/z）	子离子（m/z）	Q1预杆电压 /V	碰撞能量 /V	Q3预杆电压 /V
酮康唑	+	531.2	489.2*	-28	-31	-18
酮康唑	+	531.2	82	-28	-44	-15
氟康唑	+	307.2	220.1*	-10	-19	-15
氟康唑	+	307.2	169.1	-18	-24	-17
咪康唑	+	417.1	161.0*	-19	-32	-16
咪康唑	+	417.1	69.1	-19	-25	-26
醋酸环丙孕酮	+	417.2	279.1*	-11	-26	-13
醋酸环丙孕酮	+	417.2	147.1	-11	-25	-15
米诺地尔	+	210.2	164.1*	-19	-23	-17
米诺地尔	+	210.2	193.2	-19	-15	-20
非那雄胺	+	373.4	317.2*	-17	-24	-15
非那雄胺	+	373.4	305.2	-16	-31	-22
度他雄胺	+	529.3	461.3*	-24	-35	-23
度他雄胺	+	529.3	95.2	-24	-49	-19
RU58841	+	370.2	310.1*	-16	-21	-15
RU58841	+	370.2	352.1	-16	-16	-17
比卡鲁胺	-	429.1	225.1*	22	16	28
比卡鲁胺	-	429.1	185.1	22	39	13
尼鲁米特	-	316.1	273.1*	17	22	19
尼鲁米特	-	316.1	205.1	17	19	14

化合物	相关系数	检出限 /（μg/kg）	定量限 /（μg/kg）	回收率/%	相对标准偏差/%
米诺地尔	0.999 9	1.2	4.0	94.2	4.4
氟康唑	0.999 5	1.6	5.3	92.6	4.7
酮康唑	0.998 1	1.1	3.6	91.7	3.5
RU58841	0.999 7	1.7	5.6	90.5	2.7
尼鲁米特	0.999 2	2.4	7.9	93.1	3.1
非那雄胺	0.998 4	0.8	2.6	93.9	3.8
比卡鲁胺	0.999 3	1.9	6.3	93.7	2.3
醋酸环丙孕酮	0.994 6	1.3	4.3	91.2	3.1
咪康唑	0.998 7	2.2	7.3	92.5	3.9
度他雄胺	0.994 4	1.5	5	93.9	4.8