Determination of 35 Antibiotics in Surface Water by High Performance Liquid Chromatography-Tandem Mass Spectrometry with Online Solid-Phase Extraction and Large-Volume Injection
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摘要:
抗生素在水环境中常有检出，是国际公约管控的新污染物之一。为了控制水质和保证饮用水来源的安全使用，需要建立快速和高效的抗生素分析方法。目前能够快速测试地表水中多种类抗生素的综合分析方法有待补充。本文建立了在线固相萃取(SPE)大体积进样-高效液相色谱-串联质谱法(HPLC-MS/MS)分析地表水中9种磺胺类、16种喹诺酮类、4种大环内酯类、4种四环素类和2种其他类共35种抗生素的分析方法。根据化合物在SPE柱的保留和pH条件实验，确定莫西沙星、达氟沙星2种抗生素为碱性上样(0.1%氨水溶液)，其余33种抗生素为酸性上样(0.1%甲酸-水溶液)。采用多反应监测(MRM)扫描模式、内标法定量，35种抗生素在线性范围内的相关系数均大于0.995；方法检出限在0.1～5.2ng/L之间；在5ng/L、50ng/L和200ng/L三种加标浓度下，方法精密度分别为1.65%～12.3%、0.20%～10.4%和0.05%～9.92%；加标回收率分别为62.1%～93.1%、65.4%～127%和65.9%～124%。本方法所需样品体积小(10mL)、前处理简单，当酸性和碱性进样体积分别为3mL时，30min内能完成样品在线富集和分离分析过程。本方法应用于21件地表水样中35种抗生素的检测，林可霉素的检出率达到90.5%，氧氟沙星的检出含量最高达到98.2ng/L。本文建立的在线方法测定结果与离线方法一致，且操作简捷、灵敏度高、分析速度快，适合地表水中痕量抗生素的残留分析。
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关键词:
- 抗生素 /
- 地表水 /
- 在线固相萃取 /
- 大体积进样 /
- 高效液相色谱-串联质谱法
Abstract:Antibiotics are one of the emerging pollutants of concern in the world. Fast and efficient analytical methods for potential analysis of these pollutants are required, in order to control water quality and assure the safety of its use as a source of drinking water. However, there are few comprehensive methods to test multiple types of antibiotics in surface water. An online solid-phase extraction (SPE) of large-volume injection coupled with the high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used for the simultaneous determination of 35 antibiotics in surface water, including 9 sulfonamides, 16 quinolones, 4 macrolides, 4 tetracyclines and 2 other classes. According to compound retention in SPE column and pH condition experiments, moxifloxacin and danofloxacin were confirmed as alkaline injection (0.1% ammonia solution), while the remaining 33 antibiotics were acidic injection (0.1% formic acid solution). The analytes were detected by multiple reaction monitoring (MRM) mode and were quantified by an internal standard method. The correlation coefficients of 35 antibiotics were greater than 0.995 with the calibration concentration range from 1−500ng/L. The method limits of detection (MLD) were low, ranging between 0.1−5.2ng/L. At 3 spiked concentrations of 5ng/L, 50ng/L, and 200ng/L, the relative standard deviation (RSD) of matrix labeling (n=6) were 1.65%−12.3%, 0.2%−10.4% and 0.05%−9.92%, respectively. The recovery rate of target compounds spike in the water samples were 62.1%−93.1%, 65.4%−127% and 65.9%−124%, respectively. The developed method only required a small sample volume (10mL) and simple pretreatment. When the acidic and basic injection volume were both 3mL, the total sample run time was only 30min including sample uptake, injection, online preconcentration, and detection. The developed method was applied to the analysis of 35 antibiotics in 21 surface waters, of which the detection rate of lincomycin reached 90.5%, and the highest content of ofloxacin reached 98.2ng/L. Compared with the conventional offline detection method, the detection results of the two methods were consistent, but the online detection method was simple, sensitive, accurate and fast, and capable of the real-time detection of water samples, making it suitable for residual analysis of trace antibiotics in surface water.
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Key words:
- antibiotics /
- surface water /
- online solid-phase extraction /
- large-volume injection /
- HPLC-MS/MS
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表 1 抗生素分析中MRM优化参数、保留时间、线性相关系数和方法检出限
Table 1. MRM mass spectrum optimum parameters, retention time, linear correlation coefficient and method detection limits of antibiotic analysis
抗生素 母离子 子离子 Q1电压
(V)碰撞电压
(V)Q3电压
(V)保留时间
(min)相关系数 检出限▲
(ng/L)内标分组 林可霉素 (LIN) 407.3 126.1*/359.3 14 30 12 5.501 0.9998 0.8 2 吡哌酸 (PPA) 304.15 286.1*/215.05 14 20 13 5.540 0.9998 0.9 2 磺胺醋酰(SA) 215.05 156*/92.05 22 13 26 5.605 0.9997 0.9 2 依诺沙星 (ENO) 320.9 303*/204.05 11 22 14 6.021 0.9957 0.8 1 诺氟沙星 (NOR) 319.9 302.1*/230.95 11 24 14 6.163 0.995 2.8 1 氧氟沙星 (OFL) 362.2 318.15*/261.1 13 19 15 6.183 0.9971 1.8 3 磺胺吡唑 (SPD) 250 156*/92.05 11 16 15 6.191 0.9996 0.1 2 氟罗沙星 (FLE) 370 326*/269 10 20 15 6.210 0.9983 2.2 4 土霉素 (OTC) 461.1 426.05*/443.1 12 21 21 6.239 0.9987 2.1 4 环丙沙星 (CIP) 332.2 314.1*/231 12 22 22 6.272 0.9986 5.1 4 洛美沙星 (LOM) 352.2 265*/308.15 12 25 12 6.429 0.9966 4.9 5 四环素 (TC) 445.1 410*/427.1 12 20 19 6.527 0.9981 1.9 5 恩诺沙星 (ENR) 360.25 342.15*/316.15 13 23 16 6.538 0.9983 5.2 5 磺胺甲噻二唑 (SMTZ) 271 156*/108 18 15 30 6.858 0.9989 0.1 6 磺胺二甲嘧啶 (SM2) 279 186*/92.05 13 18 19 6.871 0.9989 0.1 6 螺旋霉素 (SPI) 843.5 174.15*/540.25 24 35 17 6.888 0.9987 0.1 6 司帕沙星 (SPR) 393 349*/292 10 20 16 6.957 0.9983 1.4 6 双氟沙星 (DIF) 400 356*/299 14 19 12 6.971 0.9983 0.2 6 磺胺对甲氧嘧啶 (SMT) 281.1 156.1*/108.1 13 17 16 7.004 0.9995 0.1 6 金霉素 (CTC) 478.8 443.95*/154.05 17 22 15 7.290 0.9991 1.2 7 强力霉素 (DOX) 444.9 428.05*/154.1 12 20 20 7.468 0.9985 2.8 7 磺胺氯哒嗪 (SCPD) 285 156*/92.05 19 15 16 7.548 0.9995 1.2 7 西诺沙星 (CIN) 263.1 245.05*/189 12 16 16 7.739 0.9992 0.3 7 磺胺邻二甲氧嘧啶 (SDO) 311 156*/108 14 18 16 7.775 0.9993 0.1 7 磺胺二甲异噁唑 (SIZ) 268 156*/92.05 12 14 27 8.011 0.9995 0.1 8 氯霉素(CAP) 321 152.1*/257 11 16 27 8.118 0.9996 0.1 8 噁喹酸 (OXA) 262.1 244.05*/216 12 19 11 8.125 0.9998 0.1 8 红霉素 (ERY) 734.3 158.15*/576.35 20 31 10 8.167 0.9987 1.1 8 磺胺间二甲氧嘧啶 (SDM) 311 156.05*/92.05 14 21 16 8.472 0.9987 0.1 8 罗红霉素 (ROX) 837.5 158.15*/679.4 222 33 16 8.952 0.9998 0.2 8 萘啶酸 (NDA) 233.1 215.05*/187 11 17 22 9.097 0.9987 0.1 8 氟甲喹 (FLU) 262.1 244.1*/202 12 20 24 9.228 0.9996 0.1 8 交沙霉素 (JOS) 828.4 174.15*/229.15 2 34 18 9.291 0.9976 0.1 8 莫西沙星 (MOX) 358.2 340.1*/225 12 23 16 7.107 0.9957 0.3 7 达氟沙星 (DAN) 402.1 245.05*/261 18 39 25 6.405 0.9979 1.0 4 噻苯达唑-D4 206 135.00*/179.1 13 33 13 5.793 — — 1 磺胺吡啶-13C6 256.05 190.05*/162.05 17 20 20 6.169 — — 2 氧氟沙星-D3 361.1 254.95*/343.1 17 40 25 6.194 — — 3 达氟沙星-D3 365.1 261.00*/321.1 17 30 17 6.395 — — 4 洛美沙星-D5 357.05 270.10*/339.05 12 24 12 6.434 — — 5 磺胺二甲嘧啶-13C6 285.05 204.05*/162.05 10 17 12 6.879 — — 6 磺胺氯哒嗪-13C6 291 162.05*/114.05 10 16 10 7.538 — — 7 氯霉素-D5 326.05 157.10*/262.15 11 17 10 8.088 — — 8 注：“*”表示定量离子；“▲”表示检出限结果是在不同的目标物浓度下得到的，检出限结果在0.1～0.3ng/L、0.8～2ng/L、2.1～2.8ng/L、4.9～5.2ng/L范围使用的目标物浓度分别为0.5ng/L、5ng/L、10ng/L和15ng/L。
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表 2 方法加标回收率和精密度实验结果(n=6)
Table 2. Precision and accuracy of the method for the determination of 35 antibiotics (n=6)
抗生素 浓度
(ng/L)加标浓度(5ng/L) 加标浓度(50ng/L) 加标浓度(200ng/L) 回收率(%) RSD(%) 回收率(%) RSD(%) 回收率(%) RSD（%） 林可霉素 (LIN) ND 65.2 8.71 67.2 8.37 68.5 7.34 吡哌酸 (PPA) ND 75.4 9.12 79.9 8.88 81.0 0.05 磺胺醋酰(SA) ND 63.7 6.43 68.2 4.41 70.5 4.26 依诺沙星 (ENO) ND 85.2 8.32 114 1.73 88.0 3.80 诺氟沙星 (NOR) ND 79.4 12.3 112 10.23 94.0 6.01 氧氟沙星 (OFL) ND 70.5 5.34 71.5 2.39 75.6 1.04 磺胺吡唑(SPD) ND 76.2 3.97 75.4 0.20 77.9 1.85 氟罗沙星 (FLE) ND 70.3 12.2 68.8 8.92 71.5 9.92 土霉素 (OTC) ND 62.1 6.85 65.4 5.87 67.7 3.40 环丙沙星 (CIP) ND 71.2 4.39 70.7 0.89 82.5 1.42 洛美沙星 (LOM) ND 75.2 9.85 77.7 6.74 85.0 1.16 四环素 (TC) ND 69.1 7.69 79.9 0.62 70.2 4.47 恩诺沙星 (ENR) ND 72.1 3.82 101 1.90 73.9 1.92 磺胺甲噻二唑 (SMTZ) ND 73.2 6.96 77.4 4.83 77.3 0.35 磺胺二甲嘧啶 (SM2) ND 80.5 3.21 82.0 1.41 76.2 1.20 螺旋霉素 (SPI) ND 76.7 8.76 81.3 4.14 81.2 0.61 司帕沙星 (SPR) ND 72.1 10.2 76.6 8.46 73.7 4.36 双氟沙星 (DIF) ND 75.3 7.64 111 2.87 73.1 3.74 磺胺对甲氧嘧啶 (SMT) ND 78.6 5.36 81.1 0.26 77.7 2.37 金霉素 (CTC) ND 65.2 9.86 67.2 8.26 65.9 7.27 强力霉素 (DOX) ND 62.1 12.1 69.8 10.36 68.7 2.51 磺胺氯哒嗪 (SCPD) ND 72.3 6.78 79.6 0.58 80.0 1.19 西诺沙星 (CIN) ND 93.1 5.74 119 3.47 124 2.37 磺胺邻二甲氧嘧啶 (SDO) ND 80.3 3.58 80.5 0.65 85.1 1.35 磺胺二甲异噁唑 (SIZ) ND 71.2 2.46 75.3 1.53 78.2 0.74 氯霉素(CAP) ND 65.1 5.64 68.6 2.99 73.5 1.56 噁喹酸 (OXA) ND 83.1 7.26 103 2.16 88.5 1.78 红霉素 (ERY) ND 85.1 8.37 127 1.91 99.1 6.40 磺胺间二甲氧嘧啶 (SDM) ND 72.3 4.56 74.5 1.69 81.6 0.12 罗红霉素 (ROX) ND 92.1 6.21 114 5.22 124 0.17 萘啶酸(NDA) ND 85.6 6.89 120 0.53 108 4.36 氟甲喹 (FLU) ND 90.3 1.65 119 0.40 93.6 0.70 交沙霉素 (JOS) ND 87.6 5.82 116 4.51 123 1.86 莫西沙星 (MOX) ND 70.3 9.65 86.9 7.84 82.8 3.30 达氟沙星 (DAN) ND 76.1 8.78 75.2 8.84 78.6 2.36 注：ND表示检测值低于检出限。
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表 3 实际样品中检出的抗生素及含量范围
Table 3. The detected antibiotics and their content ranges in samples
抗生素 在线检测 离线检测 检出样品数
(件)检出率
(%)含量范围
(ng/L)检出样品数
(件)检出率
(%)含量范围
(ng/L)林可霉素 (LIN) 19 90.5 ND～55.7 18 85.7 ND～62.1 吡哌酸 (PPA) 2 9.5 ND～48.0 2 9.5 ND～52.0 氧氟沙星 (OFL) 4 19.1 ND～98.2 4 19.1 ND～90.2 磺胺吡唑 (SPD) 8 38.1 ND～5.6 8 38.1 ND～6.1 氟罗沙星 (FLE) 4 19.1 ND～38.5 4 19.1 ND～40.2 恩诺沙星 (ENR) 2 9.5 ND～68.4 2 9.5 ND～60.4 磺胺二甲嘧啶 (SM2) 1 4.8 ND～14.3 1 4.8 ND～15.1 双氟沙星 (DIF) 5 23.8 ND～40.5 5 23.8 ND～40..5 强力霉素 (DOX) 1 4.8 ND～33.7 1 4.8 ND～36.2 磺胺氯哒嗪 (SCPD) 1 4.8 ND～5.9 1 4.8 ND～6.1 氟甲喹 (FLU) 1 4.8 ND～11.3 1 4.8 ND～12.1 莫西沙星 (MOX) 1 4.8 ND～25.8 1 4.8 ND～26.5 达氟沙星 (DAN) 1 4.8 ND～28.2 1 4.8 ND～30.1
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