HPLC-MS/MS法同时测定纺织品中八种二苯甲酮类化合物
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摘要
建立了同时测定纺织品中2-羟基-4-甲氧基二苯甲酮-5-磺酸(BP-4)、2-羟基-4-甲氧基二苯甲酮-5-磺酸钠(BP-5)、2,2′,4,4′-四羟基二苯甲酮(2,2′,4,4′OH-BP)、4-羟基二苯甲酮(4OH-BP)、2,4-二羟二苯甲酮(2,4OH-BP)、2,2′-二羟基-4-甲氧基二苯甲酮(2,2′OH-4MeO-BP)、二苯甲酮(BP)、2-羟基-4-甲氧基二苯甲酮(BP-3)等8种二苯甲酮类化合物(BPs)的超声提取-高效液相色谱-串联质谱(USE-HPLC-MS/MS)分析方法。样品经甲醇超声波提取后,采用Poroshell 120 SB-C_(18)柱(2.1 mm×100 mm,2.7μm)分离,乙腈-0.01%(体积分数)甲酸+0.000 2%甲酸铵(质量分数)水溶液为流动相梯度洗脱,电喷雾离子源电离,正、负离子多反应监测模式进行定性和定量分析,外标法定量。结果表明,8种BPs的线性相关系数(r2)均大于0.99,检出限为0.04～0.38 mg/kg,定量下限为0.13～1.25 mg/kg。加标回收率为81.0%～108.1%,相对标准偏差(RSD)为0.2%～9.7%。
A method is developed for the simultaneous determination of eight benzophenones(BPs) including 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid(BP-4), 2-hydroxy-4-methoxybenzophenone-5-sodium sulfonate(BP-5), 2,2′,4,4′-tetrahydroxybenzophenone(2,2′,4,4′OH-BP), 4-hydroxybenzophenone(4 OH-BP), 2,4-Dihydroxybenzophenone(2,4 OH-BP), 2,2′-dihydroxy-4-methoxybenzophenone(2,2′ OH-4 MeO-BP), benzophenone(BP) and 2-hydroxy-4-methoxybenzophenone(BP-3) in textiles by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with ultrasonic extraction(USE). The samples are extracted with methanol. The separation is performed on an Poroshell 120 SBC_(18) column(2.1 mm×100 mm, 2.7 μm) using 0.01%(volume fraction) formic acid with 0.000 2%(mass fraction) ammonium format and acetonitrile as mobile phase. Identification and quantification analysis is carried out by HPLC-MS/MS coupled with electrospray ionization(ESI) source in positive and negative ion mode under multiple reactions monitoring(MRM) mode. The concentration of each analyst is calibrated by the external standard method. The results indicate that the calibration curve of eight BPs show good linear relationships between peak area and certain concentration range with correlation coefficients(r2)greater than 0.99. The limits of detection are 0.04～0.38 mg/kg. The limits of quantitation are 0.13～1.25 mg/kg. The recoveries at three spiked concentration levels are in the range of 81.0%～108.1% with relative standard deviations(RSDs) of 0.2%～9.7%.
A method is developed for the simultaneous determination of eight benzophenones(BPs) including 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid(BP-4), 2-hydroxy-4-methoxybenzophenone-5-sodium sulfonate(BP-5), 2,2′,4,4′-tetrahydroxybenzophenone(2,2′,4,4′OH-BP), 4-hydroxybenzophenone(4 OH-BP), 2,4-Dihydroxybenzophenone(2,4 OH-BP), 2,2′-dihydroxy-4-methoxybenzophenone(2,2′ OH-4 MeO-BP), benzophenone(BP) and 2-hydroxy-4-methoxybenzophenone(BP-3) in textiles by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) with ultrasonic extraction(USE). The samples are extracted with methanol. The separation is performed on an Poroshell 120 SBC_(18) column(2.1 mm×100 mm, 2.7 μm) using 0.01%(volume fraction) formic acid with 0.000 2%(mass fraction) ammonium format and acetonitrile as mobile phase. Identification and quantification analysis is carried out by HPLC-MS/MS coupled with electrospray ionization(ESI) source in positive and negative ion mode under multiple reactions monitoring(MRM) mode. The concentration of each analyst is calibrated by the external standard method. The results indicate that the calibration curve of eight BPs show good linear relationships between peak area and certain concentration range with correlation coefficients(r2)greater than 0.99. The limits of detection are 0.04～0.38 mg/kg. The limits of quantitation are 0.13～1.25 mg/kg. The recoveries at three spiked concentration levels are in the range of 81.0%～108.1% with relative standard deviations(RSDs) of 0.2%～9.7%.
引文
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[11] ZHANG Z F, REN N, LI Y F, et al. Determination of benzotriazole and benzophenone UV filters in sediment and sewage sludge[J]. Environ. Sci. Technol., 2011, 45(9):3909-3916.
[2]黄方千,李强林,杨东洁,等.有机紫外线吸收剂研究进展[J].印染,2011,37(20):47-52.
[3]张晓峰,麻文效,谢影.尼龙织物的二苯甲酮-三嗪抗紫外线整理[J].印染,2016,42(18):16-20.
[4] SCHLUMPF M, COTTON B, CONSCIENCE M, et al. In vitro and in vivo estrogen city of UV screens[J]. Environ. Health Perspect.,2001, 109(3):239-244.
[5] RHODES M C, BUCHER J R, PECKHAM J C, et al. Carcinogenesis studies of benzophenone in rats and mice[J]. Food Chem.Toxicol., 2007, 45(5):843-851.
[6]毛希琴,边海涛,曲宝成.高效液相色谱法测定化妆品中17种紫外线吸收剂[J].色谱,2013,31(8):775-780.
[7] ZHANG Y F, LEE H K. Determination of ultraviolet filters in water samples by vortex-assisted dispersive liquid-liquid micro extraction followed by gas chromatography-mass spectrometry[J].J. Chromatogr. A., 2012, 1249(15):25-31.
[8] LIU Y S, YING G G, SHAREEF A, et al. Simultaneous determination of benzotriazoles and ultraviolet filters in ground water, effluent and biosolid samples using gas chromatography-tandem mass spectrometry[J]. J. Chromatogr. A., 2011, 1218(31):5328-5335.
[9]林维宣,孙兴权,马杰.液相色谱-串联质谱法同时测定防晒化妆品中的11种紫外吸收剂[J].色谱,2013,31(5):410-415.
[10]欧玮辉,唐才明,王春维,等.超高效液相色谱-串联质谱多目标分析沉积物中的微量有机紫外线吸收剂[J].分析化学,2015,43(5):734-741.
[11] ZHANG Z F, REN N, LI Y F, et al. Determination of benzotriazole and benzophenone UV filters in sediment and sewage sludge[J]. Environ. Sci. Technol., 2011, 45(9):3909-3916.