化妆品中贝美格及其盐类的高效液相色谱检测及质谱确证
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摘要
研究建立了化妆品中贝美格及其盐类的高效液相色谱分析方法及质谱确证方法。化妆品样品以甲醇为提取溶剂进行超声提取,提取液离心处理,取上清液经微孔滤膜过滤后测定。采用Symmetry C_(18)(4.6 mm×250 mm, 5μm)高效液相色谱柱进行分离测定,外标法定量。化妆品中贝美格及其盐类的方法定量限均为0.5 mg/kg,在低、中、高3个添加水平范围内平均回收率为85.1%～107.4%,相对标准偏差为3.7%～9.3%。对于疑似阳性样品,进一步采用高效液相色谱-串联质谱法进行确认分析。
An analytical method of high-performance liquid chromatography(HPLC) has been developed for the determination of bemegride and its salts in cosmetics. High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was used thereafter for the verification of these compounds. Cosmetic samples were ultrasonically extracted with methanol as extraction solvent,then centrifuged, and filtered by microporous membrane filter prior to instrumental analysis. The chromatographic separation of the analytes was performed using a Symmetry C_(18)(4.6 mm × 250 mm, 5 μm) column. The quantitation was carried out by external standard method. The experimental results indicated that the limits of quantitation(LOQ) for bemegride and its salts were all 0.5 mg/kg. The mean recoveries at three spiked levels are in the range from 85.1% to 107.4% with the relative standard deviations(RSDs) between 3.7%and 9.3%. The suspected positive samples were subjected to further verification by HPLC-MS/MS.
An analytical method of high-performance liquid chromatography(HPLC) has been developed for the determination of bemegride and its salts in cosmetics. High performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was used thereafter for the verification of these compounds. Cosmetic samples were ultrasonically extracted with methanol as extraction solvent,then centrifuged, and filtered by microporous membrane filter prior to instrumental analysis. The chromatographic separation of the analytes was performed using a Symmetry C_(18)(4.6 mm × 250 mm, 5 μm) column. The quantitation was carried out by external standard method. The experimental results indicated that the limits of quantitation(LOQ) for bemegride and its salts were all 0.5 mg/kg. The mean recoveries at three spiked levels are in the range from 85.1% to 107.4% with the relative standard deviations(RSDs) between 3.7%and 9.3%. The suspected positive samples were subjected to further verification by HPLC-MS/MS.
引文
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[16]梁婧,庄婉娥,魏丹琦.气相色谱-质谱法测定化妆品中19种邻苯二甲酸酯[J].色谱,2012,30(3):273-279.
[17]王征,韩超,游飞明.气相色谱及气相色谱-质谱法测定化妆品中的6种乙二醇醚类化合物[J].香料香精化妆品,2013,10(5):24-28.
[18]徐莉,庞道标,符灵梅,等.超高效合相色谱法测定化妆品中7种防晒剂研究[J].理化检验-化学分册,2015,51(12):1666-1669.
[19]郭项雨,马强,孟宪双,等.常压敞开式离子化-离子迁移谱法快速筛查化妆品中3种禁用卤代水杨酰苯胺[J].卫生研究,2017,46(3):467-471.
[20]闫萌萌,郭项雨,孟宪双,等.原位采样离子化-离子迁移谱法测定化妆品中5种禁用香豆素类化合物[J].日用化学工业,2017,47(9):536-540.
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[2]汤汝,董美珍,郭婷,等.参附注射液、氨茶碱、纳洛酮和贝美对老年年患者全身麻醉苏醒质量的对比研究[J].中华中医药学刊,2011,29(4):932-934.
[3]欧阳漪凡.贝美格在癫痫中临床应用[J].中国实用医药,2013,8(5):165.
[4]苑爱云,张雷红,刘秋燕.贝美格致惊大鼠海马凋亡抑制基因bcl-2表达年龄特征[J].齐鲁医学杂志,2016,31(2):177-180.
[5]王群,阮旭中,李震中.雌、孕激素对贝美格致痫大鼠大脑皮层、海马Glu和GABA免疫反应细胞的影响[J].中国组织化学与细胞化杂志,2000,9(2):214-218.
[6]中华人民共和国国家食品药品监督管理总局.化妆品安全技术规范(2015版)[S].北京:中华人民共和国国家食品药品监督管理总局,2015.
[7]郭项雨,马强,孟宪双,等.防晒类化妆品中2种帕地马酯的高效液相色谱检测及质谱确证[J].分析科学学报,2016,32(6):779-782.
[8]郭项雨,马强,孟宪双,等.化妆品中6种卤代水杨酰苯胺的高效液相色谱检测及质谱确证[J].分析试验室,2016,35(9):1033-1037.
[9]崔凤杰,故婕,张坤,等.高效液相色谱法测定化妆品中22种紫外吸收剂[J].日用化学工业,2017,41(1):52-56.
[10]马强,白桦,李文涛,等.超高效液相色谱-四极杆-飞行时间质谱法快速筛查化妆品中18种香豆素类化合物[J].分析测试学报,2014,33(3):248-255.
[11]李兆永,王凤美,牛增元,等.超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱快速筛查化妆品中的24种激素[J].色谱,2014,32(5):477-484.
[12]李强,张晓光,马俊美,等.超高效液相色谱-高分辨率质谱法筛查化妆品中12种糖皮质激素[J].分析测试学报,2016,35(2):179-184.
[13]何燕莉,王自,严小红.高效液相色谱-四极杆飞行时间串联质谱同时测定化妆品中12种紫外吸收剂[J].中国卫生检验杂志,2017,27(22):3221-3224.
[14]宋春雨,王芳,王永.气相色谱法对化妆品中防腐剂碘丙炔基丁基氨基甲酸酯的检测[J].广东化工,2017,44(9):260-261.
[15]陆军,矫筱蔓,佟晓波,等.气相色谱法同时测定化妆品中15种防腐剂[J].日用化学工业,2012,42(2):146-149.
[16]梁婧,庄婉娥,魏丹琦.气相色谱-质谱法测定化妆品中19种邻苯二甲酸酯[J].色谱,2012,30(3):273-279.
[17]王征,韩超,游飞明.气相色谱及气相色谱-质谱法测定化妆品中的6种乙二醇醚类化合物[J].香料香精化妆品,2013,10(5):24-28.
[18]徐莉,庞道标,符灵梅,等.超高效合相色谱法测定化妆品中7种防晒剂研究[J].理化检验-化学分册,2015,51(12):1666-1669.
[19]郭项雨,马强,孟宪双,等.常压敞开式离子化-离子迁移谱法快速筛查化妆品中3种禁用卤代水杨酰苯胺[J].卫生研究,2017,46(3):467-471.
[20]闫萌萌,郭项雨,孟宪双,等.原位采样离子化-离子迁移谱法测定化妆品中5种禁用香豆素类化合物[J].日用化学工业,2017,47(9):536-540.
[21]MA Q,BAI H,LI W,et al.Direct identification of prohibited substances in cosmetics and foodstuffs using ambient ionization on a miniature mass spectrometry system[J].Analytica Chimica Acta,2016,912:65-73.