超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查及定量分析保健品中29种非法添加物
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摘要
目的 建立超高效液相色谱-四极杆/静电场轨道阱质谱法(ultra performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectrometry, UPLC-Q-Orbitrap HRMS)快速筛查及定量分析保健品中常见29种非法添加物的方法。方法 样品用甲醇进行超声提取,经去离子水稀释后用UPLC-Q-Orbitrap HRMS进行测定。色谱柱选用HSS T3(1.8μm)柱,质谱采用全扫描/数据依赖二级扫描模式,通过一级质谱和二级质谱信息建立的数据库进行高通量筛查及定量分析。对建立的方法进行方法学考察,幵对市售保健品样品进行筛查测定。结果 各组分在0.1～500 ng/mL浓度范围内具有良好的线性,各化合物的检出限为0.3～20 ng/g,回收率为68.2%～105.3%,相对标准偏差为0.4%～11.3%,能够满足日常检测的要求。结论该方法简单快捷,准确度高,可用于检测保健品中非法添加物的日常监管工作。
Objective To establish a method for rapid screening and quantitative analysis of 29 kinds of illegally added compounds in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS). Methods HSS T3(1.8 μ m) column was selected for the chromatographic column, and full scan/data-dependent second-order scanning mode was adopted for the mass spectrometry, and high-throughput screening and quantitative analysis were performed using a database of primary and secondary mass spectra information. The methodology of the established method was investigated, and the samples of health care products were screened and determined. Results Each component had a good linearity in the concentration range of 0.1-500 ng/mL. The detection limits of each compound were 0.3-20 ng/g, and the recoveries were 68.2%-105.3%. The relative standard deviations were 0.4% to 11.3%, which could meet the requirements of daily detection. Conclusion This method is simple, rapid and accurate, which can be used to detect the illegal additives in health products.
Objective To establish a method for rapid screening and quantitative analysis of 29 kinds of illegally added compounds in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q-Orbitrap HRMS). Methods HSS T3(1.8 μ m) column was selected for the chromatographic column, and full scan/data-dependent second-order scanning mode was adopted for the mass spectrometry, and high-throughput screening and quantitative analysis were performed using a database of primary and secondary mass spectra information. The methodology of the established method was investigated, and the samples of health care products were screened and determined. Results Each component had a good linearity in the concentration range of 0.1-500 ng/mL. The detection limits of each compound were 0.3-20 ng/g, and the recoveries were 68.2%-105.3%. The relative standard deviations were 0.4% to 11.3%, which could meet the requirements of daily detection. Conclusion This method is simple, rapid and accurate, which can be used to detect the illegal additives in health products.
引文
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[8]Deconinck E,Verlinde K,Courselle P,et al.A validated ultra high pressure liquid chromatographic method for the characterisation of confiscated illegal slimming products containing anorexics[J].J Pharm Biom Anal,2012,59(2):38-43.
[9]李涛,朱小红,林芳.GC-MS联用方法检测降压类中成药及保健食品中非法添加的化学药物[J].药物分析杂志,2010,30(11):2212-2215.Li T,Zhu XH,Lin F.GC-MS determination of chemical drugs added illegally in Chinese patent medicine and health food[J].Chin J Pharm Anal,2010,30(11):2212-2215.
[10]谭贵良,赵天珍,王文林,等.气相色谱-质谱法同时测定腊肠中7种镇静剂类药物残留[J].现代食品科技,2014,30(2):274-278.Tan GL,Zhao TZ,Wang WL,et al.Determination of seven sedative residues in sausage by gaschromatography-mass spectrometry[J].Mod Food Sci Technol,2014,30(2):274-278.
[11]蒋丼萍,屠婕红,徐宏祥,等.UPLC-MS/MS法测定抗疲劳类保健食品中非法添加的9种壮阳类化学药物[J].中草药,2015,46(15):2238-2245.Jiang LP,Tu JH,Xu HX,et al.Determination of nine chemicals illegally added into antifatigue health foods by UPLC-MS/MS[J].Chin Tradit Herb Drug,2015,46(15):2238-2245.
[12]王颖,贾丼,朱琳娜,等.UPLC-MS/MS法同时测定保健品中11种非法添加药物[J].食品科技,2018,43(5):327-331.Wang Y,Jia L,Zhu LN,et al.Simultaneous determination of 11 illegally added drugs in healthcare foods by ultra performance liquid chromatography-tandem mass spectrometry[J].Food Sci Technol,2018,43(5):327-331.
[13]欧贝丼,张红伟,徐宏祥.UPLC-MS/MS法测定中成药及保健品中添加的36种化学药物[J].药物分析杂志,2013,33(12):2141-2147.Ou BL,Zhang HW,Xu HX.UPLC-MS/MS determination of 36chemicals added into traditional Chinese medicines and health care products[J].Chin J Pharm Anal,2013,33(12):2141-2147.
[14]柳菡,张亚莲,丁涛,等.高效液相色谱-四极杆/静电场轨道阱高分辨质谱用于葡萄酒中111种农药残留的定性筛查与定量分析[J].分析测试学报,2014,33(5):489-498.Liu H,Zhang YL,Ding T,et al.Screening and quantification of 111pesticide residues in wines by high performance liquid chromatographyquadrupole/electrostatic field orbitrap high-resolution mass spectrometry[J].J Instrum Anal,2014,33(5):489-498.
[15]董喆,李梦怡,吴迪,等.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查及定量分析减肥类保健品中20种非法添加药物[J].食品安全质量检测学报,2017,8(10):4031-4038.Dong Z,Li MY,Wu D,et al.Rapid screening and quantitative detection of20 kinds of illegally added drugs in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry[J].J Food Saf Qual,2017,8(10):4031-4038.
[16]程建桥,王传胜,张峰,等.超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法测定猪肉中氯丙嗪及其代谢物[J].食品安全质量检测学报,2018,9(10):2440-2445.Cheng JQ,Wang CS,Zhang F,et al.Determination of chlorpromazine and its metabolites in pork by ultra performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectrometry[J].J Food Saf Qual,2018,9(10):2440-2445.
[2]Liu FY,Zhang XF,Li YQ,et al.Simultaneous screening and determination of eight tetracycline antibiotics illegally adulterated in herbal preparations using HPLC-DAD combined with LC-MS-MS[J].Chromatographia,2018,81(2):303-314.
[3]徐远金,许桂苹,魏远安.毛细管电泳-质谱联用法测定性保健品中的脱水吗啡和西地那非[J].分析测试学报,2006,25(2):35-38.Xu YJ,Xu GP,Wei YA.Determination of apomorphine and sildenafil in medicines for erectile dysfunction by capillary electrophoresis-mass spectrometry[J].J Instrum Anal,2006,25(2):35-38.
[4]张宏莲,李莉,李智,等.TLC-IR法检测降糖中药及保健品中掺入2种双胍类药物[J].药物分析杂志,2013,33(12):2061-2064.Zhang HL,Li L,Li Z,et al.Identification of two kinds of biguanides illegally added to traditional Chinese medicines and health products by TLC-IR[J].Chin J Pharm Anal,2013,33(12):2061-2064.
[5]施亚琴,姚静,张启明,等.薄层色谱法快速筛查降血糖中成药及保健食品中添加磺酰脲类化学降糖药[J].药物分析杂志,2007,27(1):36-39.Shi YQ,Yao J,Zhang QM,et al.TLC method for screening sulphonylureas in antidiabetics Chinese traditional patent medicines and health supplementary foods[J].Chin J Pharm Anal,2007,27(1):36-39.
[6]张晓丹,陈静,伍小勇,等.多次进样循环使用流动相HPLC-DAD法的建立及在快速筛查消渴类中成药中非法添加化学成分中的应用[J].药物分析杂志,2011,31(6):1088-1093.Zhang XD,Chen J,Wu XY,et al.Development of HPLC-DAD method based on recycling mobile phase for mutiple sample injections and application of the method for rapid screening of chemicals illegally adulterated in traditional Chinese medicine[J].Chin J Pharm Anal,2011,31(6):1088-1093.
[7]王静文,黄湘鹭,曹进,等.超高效液相色谱法同时测定减肥类保健食品中非法添加的25种药物[J].色谱,2014,32(2):151-156.Wang JW,Huang XL,Cao J,et al.Simultaneous determination of 25illegally added drugs in diet health foods by ultra-high performance liquid chromatography[J].Chin J Chromatogr,2014,32(2):151-156.
[8]Deconinck E,Verlinde K,Courselle P,et al.A validated ultra high pressure liquid chromatographic method for the characterisation of confiscated illegal slimming products containing anorexics[J].J Pharm Biom Anal,2012,59(2):38-43.
[9]李涛,朱小红,林芳.GC-MS联用方法检测降压类中成药及保健食品中非法添加的化学药物[J].药物分析杂志,2010,30(11):2212-2215.Li T,Zhu XH,Lin F.GC-MS determination of chemical drugs added illegally in Chinese patent medicine and health food[J].Chin J Pharm Anal,2010,30(11):2212-2215.
[10]谭贵良,赵天珍,王文林,等.气相色谱-质谱法同时测定腊肠中7种镇静剂类药物残留[J].现代食品科技,2014,30(2):274-278.Tan GL,Zhao TZ,Wang WL,et al.Determination of seven sedative residues in sausage by gaschromatography-mass spectrometry[J].Mod Food Sci Technol,2014,30(2):274-278.
[11]蒋丼萍,屠婕红,徐宏祥,等.UPLC-MS/MS法测定抗疲劳类保健食品中非法添加的9种壮阳类化学药物[J].中草药,2015,46(15):2238-2245.Jiang LP,Tu JH,Xu HX,et al.Determination of nine chemicals illegally added into antifatigue health foods by UPLC-MS/MS[J].Chin Tradit Herb Drug,2015,46(15):2238-2245.
[12]王颖,贾丼,朱琳娜,等.UPLC-MS/MS法同时测定保健品中11种非法添加药物[J].食品科技,2018,43(5):327-331.Wang Y,Jia L,Zhu LN,et al.Simultaneous determination of 11 illegally added drugs in healthcare foods by ultra performance liquid chromatography-tandem mass spectrometry[J].Food Sci Technol,2018,43(5):327-331.
[13]欧贝丼,张红伟,徐宏祥.UPLC-MS/MS法测定中成药及保健品中添加的36种化学药物[J].药物分析杂志,2013,33(12):2141-2147.Ou BL,Zhang HW,Xu HX.UPLC-MS/MS determination of 36chemicals added into traditional Chinese medicines and health care products[J].Chin J Pharm Anal,2013,33(12):2141-2147.
[14]柳菡,张亚莲,丁涛,等.高效液相色谱-四极杆/静电场轨道阱高分辨质谱用于葡萄酒中111种农药残留的定性筛查与定量分析[J].分析测试学报,2014,33(5):489-498.Liu H,Zhang YL,Ding T,et al.Screening and quantification of 111pesticide residues in wines by high performance liquid chromatographyquadrupole/electrostatic field orbitrap high-resolution mass spectrometry[J].J Instrum Anal,2014,33(5):489-498.
[15]董喆,李梦怡,吴迪,等.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查及定量分析减肥类保健品中20种非法添加药物[J].食品安全质量检测学报,2017,8(10):4031-4038.Dong Z,Li MY,Wu D,et al.Rapid screening and quantitative detection of20 kinds of illegally added drugs in diet health foods by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry[J].J Food Saf Qual,2017,8(10):4031-4038.
[16]程建桥,王传胜,张峰,等.超高效液相色谱-四级杆/静电场轨道阱高分辨质谱法测定猪肉中氯丙嗪及其代谢物[J].食品安全质量检测学报,2018,9(10):2440-2445.Cheng JQ,Wang CS,Zhang F,et al.Determination of chlorpromazine and its metabolites in pork by ultra performance liquid chromatographyquadrupole/electrostatic field orbitrap high resolution mass spectrometry[J].J Food Saf Qual,2018,9(10):2440-2445.