A sensitive and selective method was developed and validated for the determination of 26 anticoccidial compounds (six ionophores and twenty chemical coccidiostats) in surface and groundwater samples at parts-per-quadrillion (pg L-1) to parts-per-trillion (ng L-1) levels by ultra-high performance liquid chromatography with tandem mass spectrometry detection (UHPLC-MS/MS). A range of different analytical columns and mobile phase compositions were evaluated to enhance selectivity and retention of a number of highly polar and basic anticoccidials along with other non-polar coccidiostats. A combined separation, including these problematic polar compounds, was achieved on a phenyl-hexyl column, by binary gradient elution with water/acetonitrile using ammonium formate and formic acid as additives. The anticoccidial residues were extracted from raw, unfiltered, water samples (250 mL) using polymeric divinylbenzene solid phase extraction (SPE) cartridges, with subsequent elution (methanol:acetonitrile:ethyl acetate, 40:40:20, v/v) and concentration prior to determination. The method recovery (at a concentration representative of realistic expected environmental water concentrations based on literature review) ranged from 81% to 105%. The method was successfully validated for 26 anticoccidials, at four concentration levels, in accordance to Commission Decision 2002/657/EC and SANTE/11813/2017 guidelines. Trueness and precision, under within-laboratory reproducibility conditions, ranged from 88% to 111% and 0.9% to 10.3% respectively.

中文翻译：

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一种同时进行色谱分离和串联质谱检测环境水中抗球虫药（包括高极性化合物）的灵敏的新方法。

开发了一种灵敏且选择性的方法，用于测定地表水和地下水样品中的26种抗球虫化合物（6种离子载体和20种化学抗球虫药），其测定方法为百万分之几（pg L-1）至万亿分之几（ng L -1）通过串联质谱检测的超高效液相色谱（UHPLC-MS / MS）测定。评估了各种不同的分析柱和流动相的组成，以提高许多高极性和碱性抗球虫药以及其他非极性抗球虫药的选择性和保留率。通过使用甲酸铵和甲酸作为添加剂的水/乙腈二元梯度洗脱，在苯基己基色谱柱上实现了包括这些有问题的极性化合物在内的组合分离。抗球虫病残留物是从原料中提取的，使用聚合的二乙烯基苯固相萃取（SPE）小柱过滤未过滤的水样品（250 mL），随后进行洗脱（甲醇：乙腈：乙酸乙酯，40:40:20，v / v）和浓缩，然后测定。方法的回收率（根据文献综述以代表实际预期环境水浓度的浓度表示）为81％至105％。根据委员会决定2002/657 / EC和SANTE / 11813/2017指南，该方法已成功验证了四个浓度水平下的26种抗球虫药。在实验室内可重复性条件下，真实度和精确度分别为88％至111％和0.9％至10.3％。40：40：20，v / v）和浓度后再测定。方法的回收率（根据文献综述以代表实际预期环境水浓度的浓度表示）为81％至105％。根据委员会决定2002/657 / EC和SANTE / 11813/2017准则，该方法已成功验证了四个浓度水平下的26种抗球虫药。在实验室内可重复性条件下，真实度和精确度分别为88％至111％和0.9％至10.3％。40：40：20，v / v）和浓度后再测定。方法的回收率（根据文献综述以代表实际预期环境水浓度的浓度表示）为81％至105％。根据委员会决定2002/657 / EC和SANTE / 11813/2017指南，该方法已成功验证了四个浓度水平下的26种抗球虫药。在实验室内可重复性条件下，真实度和精确度分别为88％至111％和0.9％至10.3％。根据委员会决定2002/657 / EC和SANTE / 11813/2017准则进行。在实验室内可重复性条件下，真实度和精确度分别为88％至111％和0.9％至10.3％。根据委员会决定2002/657 / EC和SANTE / 11813/2017准则进行。在实验室内可重复性条件下，真实度和精确度分别为88％至111％和0.9％至10.3％。