HPLC-MS/MS Determination of Minoxidil of Illegal Addition in Cosmetics
摘 要
采用高效液相色谱-串联质谱法测定化妆品中非法添加的米诺地尔的含量。样品以饱和氯化钠溶液盐析破乳,用乙腈超声提取20 min,离心后,取上清液过0.22 μm滤膜。以ACQUITY UPLC® BEH C18色谱柱为固定相,以不同体积比的0.2%(体积分数,下同)乙酸溶液和0.2%乙酸甲醇溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾正离子源和多反应监测模式,采用同位素内标法定量。米诺地尔的线性范围为5~500 μg·L-1,检出限(3S/N)为1 ng·g-1。以空白样品为基体进行加标回收试验,所得回收率为108%~114%,回收量的相对标准偏差(n=6)为1.2%~2.8%。
Abstract
HPLC-MS/MS was applied to the determination of minoxidil of illegal addition in cosmetics. Saturated sodium chloride solution was added in the sample for salting out and demulsification. The sample solution was extracted ultrasonically for 20 min with acetonitrile. After centrifugation, the supernatant was filtered on 0.22 μm filtering membrane. ACQUITY UPLC® BEH C18 chromatographic column was used as stationary phase, and the mixture of 0.2% (φ, the same below) acetic acid solution and 0.2% acetic acid methanol solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Isotope was used as internal standard. Linearity range of minoxidil were found in the range of 5-500 μg·L-1 with detection limit (3S/N) of 1 ng·g-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 108%-114%, with RSDs (n=6) of recovery amounts in the range of 1.2%-2.8%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201902012
所属栏目 工作简报
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收稿日期 2018/4/20
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备注牛水蛟,主管药师,硕士,研究方向为化妆品、保健食品检验
引用该论文: NIU Shuijiao,YU Haiying,LI Qiyan,WANG Xiaobing,LI Junjie,WU Jing. HPLC-MS/MS Determination of Minoxidil of Illegal Addition in Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(2): 193~196
牛水蛟,于海英,李启艳,王小兵,李俊婕,吴景. 高效液相色谱-串联质谱法测定化妆品中非法添加的米诺地尔[J]. 理化检验-化学分册, 2019, 55(2): 193~196
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参考文献
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【2】SINCLAIR R D. Female pattern hair loss:A pilot study investigating combination therapy with low-dose oral minoxidil and spironolactone[J]. International Journal of Dermatology, 2018,57(1):104-109.
【3】宫芮.5%与2%米诺地尔治疗雄激素性脱发疗效临床观察比较[J].山西医药杂志, 2014,43(9):1044-1046.
【4】CHOI N, SHIN S, SONG S, et al. Minoxidil promotes hair growth through stimulation of growth factor release from adipose-derived stem cells[J]. International Journal of Molecular Sciences, 2018,19(3):691-705.
【5】SAKITA S, KAGOURA M, TOYODA M, et al. The induction by topical minoxidil of increased fenestration in the perifollicular capillary wall[J]. British Journal of Dermatology, 1999,140(2):294-296.
【6】吴桥芳,范卫新.米诺地尔治疗雄激素性秃发的机制和剂型研究进展[J].临床皮肤科杂志,2018,47(2):128-131.
【7】ROGERS N E, AVRAM M R. Medical treatments for male and female pattern hair loss[J]. Journal of the American Academy of Dermatology, 2008,59(4):547-566.
【8】国家食品药品监督管理总局.化妆品安全技术规范[M].北京:国家食品药品监督管理总局, 2015.
【9】唐丽丽,谭小勇,陈华龙.育发健康产品中米诺地尔的薄层色谱快筛方法研究[J].海峡药学, 2016,28(9):77-78.
【10】国家药典委员会.中华人民共和国药典(二部)[M].北京:中国医药科技出版社, 2015.
【11】莫玉芳,叶延武.紫外分光光度法测定米诺地尔洗剂中米诺地尔的含量[J].广东药学, 2004,14(5):18-20.
【12】龚越强,吕冠欣.HPLC测定中草药育发类化妆品中非法添加的米诺地尔[J].食品与药品, 2014,16(4):267-269.
【13】管继萍,王国团,程立华.高效液相色谱法测定米诺地尔洗剂的含量[J].中国医院药学杂志, 2006,26(10):1298-1298.
【14】邓莉,林彩,胡斌,等.高效液相色谱法测定生发素中米诺地尔含量[J].药物鉴定, 2011,20(3):18-19.
【15】李佳,张涛,何德云,等.HPLC法测定斑秃搽剂中米诺地尔的含量[J].解放军药学学报, 2013,29(6):528-528.
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