为了评估育发液中是否违法添加糖皮质激素,采用超高效液相色谱串联三重四极杆质谱（UPLC-MS/MS）建立了一种同时测定育发液中35种糖皮质激素的方法。样品加饱和氯化钠溶液分散,经乙腈提取,以PRiME HLB固相萃取柱净化,ACQUITY BEH C18柱（1.7 μm,2.1 mm×100 mm）分离,流动相A为含0.1%甲酸和2 mmol/L乙酸铵的水溶液,流动相B为含0.1%甲酸的乙腈溶液,进行梯度洗脱,多反应监测模式（MRM）进行检测,外标法定量。结果表明, 35种糖皮质激素的色谱分离效果良好,在2~30 ng/mL范围内呈良好的线性关系,决定系数（R2）均大于0.99,方法检出限（LOD,S/N≥3）和定量限（LOQ,S/N≥10）分别在0.01~0.65 µg/L和0.03~2.20 µg/L之间,各加标水平的平均回收率在62.4%~92.9%之间,相对标准偏差（RSD）为1.7%~5.7%。该方法同时检测育发液中35种糖皮质激素,可用于育发液质量安全的监控。
Hair-rearing solutions is a cosmetic product that promotes hair growth, produces new hair and prevents hair loss. More and more people are suffering from hair loss problems in our country. There is a huge profit space in the market of hair growth products at home and abroad, and behind the rising for market profits, the quality problem of hair-rearing solutions often exists. For enhancing the efficacy of hair care products, the illegal drugs are added, which are mainly glucocorticoids. There are many side effects after the use of glucocorticoids, which include obesity, osteoporosis, hyperglycemia, hyperlipidemia, the appearance of acne, hirsutism, atrophic lines, etc. So the medical community at home and abroad takes the use of glucocorticoids extremely seriously. Meanwhile, glucocorticoids have been listed as prohibited substances for cosmetics in statutory standards. In recent years, glucocorticoids are being abused by some manufacturers and beauty salons as ingredients for hair loss prevention and hair growth, which leads to disruption of the hormonal balance and causes various diseases. Currently, there is no literature on determination of glucocorticoids in hair-rearing solutions. In order to assess the glucocorticoids in hair-rearing solutions, a comprehensive analytical method was developed for qualitative and quantitative determination of 35 glucocorticoids in hair-rearing solutions by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry （UPLC-MS/MS）. The sample was dispersed with saturated sodium chloride and extracted by acetonitrile, then purified with PRiME HLB. The chromatographic separation was performed on an ACQUITY BEH C18 chromatographic column（1.7 μm, 2.1 mm×100 mm）, with 0.1% formic acid and 2 mmol/L ammonium acetate of water and 0.1% formic acid of acetonitrile as mobile phases by gradient elution. The multiple reaction monitoring （MRM） acquisition mode was used for detection, and external standard method was used for quantitative detection. Results show that this method exhibits a perfect performance in chromatographic separation. The calibration curves for analytes are of good linearities in concentration ranges of 2-30 ng/mL with the coefficient of determination （R2） no less than 0.99. The limit of detection （LOD, S/N≥3） and quantitation （LOD, S/N≥10） are in the ranges of 0.01-0.65 µg/L and 0.03-2.20 µg/L, respectively. The spiked average recoveries for analytes at their spiked levels are in the range of 62.4%-92.9%, and RSD are 1.7%-5.7%. The method can simultaneously detect 35 glucocorticoids in hair-rearing solutions and can be used to monitor the quality and safety of hair-rearing solutions.
