UPLC-MS/MS Determination of 22 Forbidden Sedative-Hypnotics in Sleep-Aiding Health Care Products with SPE Column Purification
摘 要
应用超高效液相色谱-串联质谱法测定了助眠类保健品中22种禁用安神类药物的含量。将样品连同其包衣和胶囊壳一起研碎后称取1.000 g样品用甲醇溶解,经涡旋混匀并超声15 min,用甲醇定容至25.0 mL。离心后取上清液5.00 mL,经Oasis PRiME HLB固相萃取柱净化处理,收集经净化的流出液,与用于淋洗固相萃取柱的甲醇2 mL合并,于40℃下吹氮至溶液近干。用体积比为1:1的0.05%(体积分数,下同)甲酸-甲醇混合溶液1.00 mL溶解残渣,所得溶液经过0.22 μm滤膜过滤,滤液供色谱分离。选用Poroshell 120 EC-C18色谱柱(50 mm×3.0 mm,2.7 μm)作为固定相,用不同比例的(A)含0.05%甲酸的5 mmol·L-1乙酸铵溶液和(B)乙腈的混合溶液作为流动相按程序进行梯度洗脱。质谱测定中采用电喷雾离子源和多反应监测模式。结果表明:22种禁用安神类药物的标准曲线中有17种线性范围为4~800 μg·L-1,有1种为40~8 000 μg·L-1,还有4种为400~80 000 μg·L-1,其检出限(3S/N)为0.02~2 μg·g-1。用标准加入法进行回收试验,测得回收率为81.2%~98.9%,测定值的相对标准偏差(n=6)为3.1%~9.7%。
Abstract
UPLC-MS/MS was applied to the determination of 22 forbidden sedative-hypnotics in some sleep-aiding health care products. Sample for analysis was prepared by grinding the health care food itself together with its capsula into powder and a portion of 1.000 g was taken and dissolved in methanol with aid of ultrasonic treatment for 15 min. The solution was diluted to 25.0 mL with methanol and centrifuged. An aliquot of 5.00 mL of the supernatant was taken and purified by passing through the Oasis PRiME HLB SPE column. The eluate from the SPE column was collected and mixed with the methanol (2 mL) used in washing the column. The mixed solution was then evaporated to neardryness by N2-blowing at 40℃. The residue was taken up with 1.00 mL of a mixed solution of 0.005% (volume fraction, same as below) formic acid-methanol with the volume ratio of 1:1, and the solution was filtered through 0.22 μm filtering membrane and the filtrate was used for UPLC separation by passing through Poroshell 120 EC-C18 chromatographic column (50 mm×3.0 mm, 2.7 μm) as stationary phase, and mixture of (A) 5 mmol·L-1 NH4OAc solution (containting 0.05% formic acid) and (B) acetonitrile in various ratios were used as mobile phases in gradient elution. In MS/MS determination, ESI and MRM mode were adopted. It was shown that among the standard curves of the 22 forbidden sedative-hypnotics, linearity ranges for 17 sedative-hypnotics were same between 4 μg·L-1 and 800 μg·L-1, for one sedative-hypnotic between 40 μg·L-1 and 8 000 μg·L-1 and for the remaider 4 sedative-hypnotics between 400 μg·L-1 and 80 000 μg·L-1; the detection limits (3S/N) found for these sedative-hypnotics were in the range of 0.02-2 μg·g-1. Recovery was tested by standard addition method, giving values of recovery in the range of 81.2%-98.9%, and values of RSDs (n=6) in the range of 3.1%-9.7%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202001001
所属栏目 试验与研究
基金项目 浙江省分析测试科技计划项目(2018C37027)
收稿日期 2019/4/23
修改稿日期
网络出版日期
作者单位点击查看
备注钟世欢,研究方向为食品安全,244665407@qq.com
引用该论文: ZHONG Shihuan,JIN Jianqi,YE Leihai,YE Jiaming,WANG Xiao,QIU Juntao. UPLC-MS/MS Determination of 22 Forbidden Sedative-Hypnotics in Sleep-Aiding Health Care Products with SPE Column Purification[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(1): 1~6
钟世欢,金建奇,叶磊海,叶佳明,王潇,裘钧陶. 固相萃取柱净化-超高效液相色谱-串联质谱法测定助眠类保健品中22种禁用安神类药物的含量[J]. 理化检验-化学分册, 2020, 56(1): 1~6
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】ROTH T, COULOUVRAT C, HAJAK G, et al. Prevalence and perceived health associated with insomnia based on DSM-IV-TR; international statistical classification of diseases and related health problems, tenth revision; and research diagnostic criteria/international classification of sleep disorders, second edition criteria: Results from the America insomnia survey[J]. Biological Psychiatry, 2011,69(6):592-600.
【2】陆林.关注心血管疾病合并失眠障碍[J].中华内科杂志, 2017,56(4):249-249.
【3】LI M, ZHANG X W, HOU W S, et al. Insomnia and risk of cardiovascular disease: A meta-analysis of cohort studies[J]. International Journal of Cardiology, 2014,176(3):1044-1047.
【4】GRANDNER M A, Alfonso M P, FEMANDEZ M J, et al. Sleep:Important considerations for the prevention of cardiovascular disease[J]. Current Opinion in Cardiology, 2016,31(5):551-565.
【5】顾平,王淑君.失眠障碍的治疗[J].医学与哲学(B), 2017,38(10):22-25.
【6】孙烨琨,师乐,陈斯婧,等.镇静催眠药物治疗对失眠患者认知功能的影响[J].中国神经精神疾病杂志, 2017,43(11):701-704.
【7】VERGER P, AULAGIER M, PROTOPOPESCU C, et al. Hypnotic and tranquillizer use among general practitioners in south-eastern France and its relation to occupational characteristics and prescribing habits[J]. Fundamental and Clinical Pharmacology, 2004,18(3):379-385.
【8】韩东岐,鲁艺,殷果,等.HPLC-DAD法同时检测镇静安神类中成药及保健食品中非法添加的药物[J].中成药, 2015,37(10):2197-2202.
【9】李世忠,刘艳英,周扬霞.试析数字对照品法检测镇静安神类中成药和保健食品中非法添加的5种西药成分[J].中国医药指南, 2013(15):468-468.
【10】肖丽和,刘吉金,关潇滢,等.镇静安神类中成药及保健食品中非法添加化学成分的快速筛查方法研究[J].中国当代医药, 2009,16(14):15-16.
【11】WEI J M, LUO Y Z, ZHANG L, et al. Determination of 15 sedative residues in mutton by rapid resolution liquid chromatography-tandem mass spectrometry[J]. Journal of the Science of Food and Agriculture, 2015,95(3):598-606.
【12】刘家阳,黄旭,贾宏新.固相萃取/超高效液相色谱-串联质谱法测定畜肉中16种镇静剂类兽药残留[J].分析测试学报, 2017,36(3):305-311.
【13】冯雪伊,陈航,沈敏,等.微波辅助提取/液相色谱-串联质谱法同时测定人体指甲中14种抗精神失常及安眠镇静类物质[J].分析测试学报, 2016,35(10):1233-1240.
【14】LEE J H, PARK H N, CHOI J Y, et al. Simultaneous analysis by quadrupole-orbitrap mass spectrometry and UHPLC-MS/MS for the determination of sedative-hypnotics and sleep inducers in adulterated products[J]. Journal of Separation Science, 2017,40(24):4677-4688.
【2】陆林.关注心血管疾病合并失眠障碍[J].中华内科杂志, 2017,56(4):249-249.
【3】LI M, ZHANG X W, HOU W S, et al. Insomnia and risk of cardiovascular disease: A meta-analysis of cohort studies[J]. International Journal of Cardiology, 2014,176(3):1044-1047.
【4】GRANDNER M A, Alfonso M P, FEMANDEZ M J, et al. Sleep:Important considerations for the prevention of cardiovascular disease[J]. Current Opinion in Cardiology, 2016,31(5):551-565.
【5】顾平,王淑君.失眠障碍的治疗[J].医学与哲学(B), 2017,38(10):22-25.
【6】孙烨琨,师乐,陈斯婧,等.镇静催眠药物治疗对失眠患者认知功能的影响[J].中国神经精神疾病杂志, 2017,43(11):701-704.
【7】VERGER P, AULAGIER M, PROTOPOPESCU C, et al. Hypnotic and tranquillizer use among general practitioners in south-eastern France and its relation to occupational characteristics and prescribing habits[J]. Fundamental and Clinical Pharmacology, 2004,18(3):379-385.
【8】韩东岐,鲁艺,殷果,等.HPLC-DAD法同时检测镇静安神类中成药及保健食品中非法添加的药物[J].中成药, 2015,37(10):2197-2202.
【9】李世忠,刘艳英,周扬霞.试析数字对照品法检测镇静安神类中成药和保健食品中非法添加的5种西药成分[J].中国医药指南, 2013(15):468-468.
【10】肖丽和,刘吉金,关潇滢,等.镇静安神类中成药及保健食品中非法添加化学成分的快速筛查方法研究[J].中国当代医药, 2009,16(14):15-16.
【11】WEI J M, LUO Y Z, ZHANG L, et al. Determination of 15 sedative residues in mutton by rapid resolution liquid chromatography-tandem mass spectrometry[J]. Journal of the Science of Food and Agriculture, 2015,95(3):598-606.
【12】刘家阳,黄旭,贾宏新.固相萃取/超高效液相色谱-串联质谱法测定畜肉中16种镇静剂类兽药残留[J].分析测试学报, 2017,36(3):305-311.
【13】冯雪伊,陈航,沈敏,等.微波辅助提取/液相色谱-串联质谱法同时测定人体指甲中14种抗精神失常及安眠镇静类物质[J].分析测试学报, 2016,35(10):1233-1240.
【14】LEE J H, PARK H N, CHOI J Y, et al. Simultaneous analysis by quadrupole-orbitrap mass spectrometry and UHPLC-MS/MS for the determination of sedative-hypnotics and sleep inducers in adulterated products[J]. Journal of Separation Science, 2017,40(24):4677-4688.
相关信息