LC-MS/MS Determination of 15 Sex Hormones in Cosmetics
摘 要
采用液相色谱-串联质谱法(LG-MS/MS)测定了化妆品(膏霜、乳液或水剂)中15种性激素的含量。样品(0.20 g)与饱和氯化钠溶液(2 mL)混匀分散,用乙腈(每次2 mL)提取2次。合并提取液,加入200 g·L-1亚铁氰化钾溶液和200 g·L-1乙酸锌溶液各0.2 mL,混匀使大分子物质沉淀,离心后取上清液,加水定容至10 mL。按不同的程序分别对雌激素、雄激素和孕激素进行梯度洗脱。质谱测定中对雌激素采用负离子模式,雄激素和孕激素采用正离子模式。15种性激素的质量浓度均在8.0~800 μg·L-1内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.05~0.4 mg·kg-1。经多批实样分析,所得测定值的相对标准偏差(n=6)为0.90%~4.3%,加标回收率为80.3%~121%。
Abstract
LC-MS/MS was applied to the determination of 15 sex hormones in cosmetics (cream, emulsion or water preparation). The sample (0.20 g) was dispersed in 2 mL of saturated NaCl solution and extracted twice with acetonitrile (2 mL each). 0.2 mL of each of the solution of 200 g·L-1 K4Fe(CN)6 and 200 g·L-1 (CH3COO)2Zn were added to the combined extract to precipitate the large molecular matrix. After centrifugation, the supernatant was taken and its volume was made up to 10 mL. Different programs were used in the gradient elution of estrogen hormones, male hormones and progestin hormones respectively, and in MS/MS analysis, the mode of ESI- was applied to estrogen hormones and ESI+ was applied to male hormones and progestin hormones. Linear relationships between values of peak area and mass concentration of the 15 sex hormones were kept in the same range of 8.0-800 μg·L-1, with detection limits (3S/N) in the range of 0.05-0.4 mg·kg-1. Substantial samples of different batches were analyzed by this method, giving values of RSD's (n=6) in the range of 0.90% to 4.3%, and of recovery ranged from 80.3% to 121%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201802008
所属栏目 工作简报
基金项目 广州市越秀区科技计划项目(2016-PT-004);广东省省级科技计划项目(2015A030401062);广东省食品药品检验检测技术创新专项资金项目(2015ZX01)
收稿日期 2017/3/13
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备注周智明(1985-),女,江西吉安人,主管药师,硕士,研究方向为化妆品检测方法
引用该论文: ZHOU Zhiming,LUO Zhuoya. LC-MS/MS Determination of 15 Sex Hormones in Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 161~166
周智明,罗卓雅. 液相色谱-串联质谱法测定化妆品中15种性激素[J]. 理化检验-化学分册, 2018, 54(2): 161~166
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【13】于慧娟,张珊珊,张晓玲,等.同位素稀释-液相色谱-串联质谱法同时测定水产品中雌激素、孕激素和雄激素[J].质谱学报, 2014,352(2):170-178.
【2】王伟萍,张明玥,蔺娟,等.超高效液相色谱-串联质谱法同时测定化妆品中21种糖皮质激素[J].药物分析杂志, 2013,33(5):837-843.
【3】陈溪,张晓林,刘莹,等.液相色谱-串联质谱法测定化妆品中22种激素[J].理化检验-化学分册, 2013,49(4):468-476.
【4】王珊,李琼,武晓剑,等.高效液相色谱法测定化妆品中5种性激素[J].理化检验-化学分册, 2014,50(3):333-337.
【5】赵珊,吴大南,王鹏.高效液相色谱法同时测定化妆品中7种性激素[J].色谱, 2004,22(3):267-269.
【6】王君,林少彬.化妆品中性激素的分析方法研究进展[J].医学研究杂志, 2007,36(3):89-91.
【7】吴维群,沈朝烨,杨玉林,等.GC/MS联用技术检测水性化妆品中性激素成分的方法研究[J].环境与职业医学, 2004,21(4):307-309.
【8】邴爱英,成连贵,褚新星,等.己烯雌酚酶联免疫检测方法的建立[J].西南农业学报, 2006,19(6):1159-1161.
【9】赵新宇,王权,闫叶娜.建立水产品中己烯雌酚残留ELISA检测方法[J].中国畜牧兽医, 2010,37(10):43-47.
【10】赵怀鑫,孙志伟,夏莲,等.新型荧光衍生试剂用于尿样中痕量游离雌二醇和雌三醇的反相高效液相色谱-荧光检测和质谱定性[J].色谱, 2009,27(2):164-168.
【11】王超,马强,王星,等.液相色谱-串联质谱法同时测定化妆品中的16种激素[J].分析化学, 2007,35(9):1257-1262.
【12】DE ORSI D, PELLEGRINI M. High-performance liquid chromatography-diode array and electrospray-mass spectrometry analysis of non-allowed substances in cosmetic products for preventing hair loss and other hormone-dependent skin diseases[J]. Journal of Pharmaceutical and Biomedical Analysis, 2008,48:641-648.
【13】于慧娟,张珊珊,张晓玲,等.同位素稀释-液相色谱-串联质谱法同时测定水产品中雌激素、孕激素和雄激素[J].质谱学报, 2014,352(2):170-178.
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