Kasprzyk-Hordern Barbara, Dinsdale Richard M, Guwy Alan J
University of Glamorgan, Sustainable Environment Research Centre, Pontypridd CF37 1DL, UK.
Talanta. 2008 Feb 15;74(5):1299-312. doi: 10.1016/j.talanta.2007.08.037. Epub 2007 Sep 6.
A new multi-residue method for the determination of 25 acidic/neutral pharmaceuticals (antibiotics, anti-inflammatory/analgesics, lipid regulating agents, diuretics, triazides, H2-receptor antagonists, cardiac glicozides and angiotensin II antagonists) and personal care products (sunscreen agents and preservatives) in surface water with the usage of a new technique: ultra performance liquid chromatography-negative electrospray tandem mass spectrometry (UPLC-MS/MS) was developed and validated. The novel UPLC system with 1.7 microm particle-packed column allowed for good resolution of analytes with the application of low mobile phase flow rates (0.05 mL min(-1)) and short retention times (from 4.7 min to 13.3 min) delivering a fast and cost-effective multi-residue method. SPE with the usage of Oasis MCX strong cation-exchange mixed-mode polymeric sorbent was chosen for sample clean-up and concentration. The influence of mobile-phase composition, matrix assisted ion suppression and SPE recovery on the sensitivity of the method was identified and quantified. The instrumental limits of quantification varied from 0.2 microgL(-1) to 30mugL(-1). The method limits of quantification were at low nanogram per litre levels and ranged from 0.3 ng L(-1) to 30 ng L(-1). The instrumental and method intra-day and inter-day repeatabilities were on average less than 5%. The method was successfully applied for the determination of PPCPs in River Taff. Thirteen compounds were determined in river water at levels ranging from a single to a few hundred nanograms per litre. Among them were ten pharmaceuticals (aspirin, salicylic acid, ketoprofen, naproxen, diclofenac, ibuprofen, mefenamic acid, furosemide, sulfasalazine and valsartan) and three personal care products (methyl- and ethylparaben and 4-benzophenone).
采用超高效液相色谱 - 负电喷雾串联质谱法(UPLC-MS/MS)这一新技术,开发并验证了一种用于测定地表水中25种酸性/中性药物(抗生素、抗炎/镇痛药、脂质调节剂、利尿剂、三氮唑类、H2受体拮抗剂、强心苷类和血管紧张素II拮抗剂)及个人护理产品(防晒剂和防腐剂)的新型多残留方法。配备1.7微米填充柱的新型UPLC系统,通过采用低流动相流速(0.05 mL min(-1))和较短保留时间(4.7分钟至13.3分钟),实现了分析物的良好分离,从而提供了一种快速且经济高效的多残留方法。选用使用Oasis MCX强阳离子交换混合模式聚合物吸附剂的固相萃取法进行样品净化和浓缩。确定并量化了流动相组成、基质辅助离子抑制和固相萃取回收率对该方法灵敏度的影响。仪器定量限在0.2 microgL(-1)至30mugL(-1)之间。方法定量限处于低纳克每升水平,范围为0.3 ng L(-1)至30 ng L(-1)。仪器和方法的日内和日间重复性平均小于5%。该方法成功应用于塔夫河中药物和个人护理产品的测定。在河水中测定了13种化合物,浓度范围为每升单纳克至几百纳克。其中包括10种药物(阿司匹林、水杨酸、酮洛芬、萘普生、双氯芬酸、布洛芬、甲芬那酸、呋塞米、柳氮磺胺吡啶和缬沙坦)和3种个人护理产品(对羟基苯甲酸甲酯和乙酯以及二苯甲酮)。