Development of a pH-paralleling approach of quantifying six-category pharmaceuticals in surface water using SPE-HPLC-MS/MS

Bing Hong , Shen Yu , Min Zhou , Juan Li , Jing Ding , Yong Niu
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引用次数: 3

Abstract

An analytical protocol was developed to quantify six-category pharmaceuticals in surface water under paralleling pHs using a combination of solid phase extraction (SPE) and high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Of 121 compound standards commercially, 94 compounds were reliably quantified using a paralleling pH combination at 3 and 9 with a sound recovery-rate of 50-150%. The quantified compounds covered 6 categories as 37 antibiotics, 16 central nervous system drugs (CNs), 14 cardiovascular drugs (CVs), 12 endocrine and family planning drugs (EFs), 8 antiparasitic drugs (APs), and 7 non-steroidal anti-inflammatory drugs (NSAIDs). The protocol achieved limits of detection and quantitation in ranges of 0.001–11.9 ng L–1 and 0.003–39.7 ng L–1, respectively. Serial field surface water samples from Jiulong River in Fujian, China were testified using the protocol with 41 quantified compounds of the above-mentioned 6 categories from < LODs to 1,389 ng L−1 (caffeine). The key procedure prior to the SPE is to split filtrate of each surface water sample into two portions, adjusted to pH 3 and 9 separately and both spiked with 0.2 g Na2EDTA.

采用SPE-HPLC-MS/MS方法定量地表水中六类药物的ph平行方法的建立
采用固相萃取(SPE)和高效液相色谱串联质谱(HPLC-MS/MS)相结合的方法,在平行ph值条件下对地表水中的6类药物进行定量分析。在121种商业标准化合物中,94种化合物使用3和9的平行pH组合可靠地定量,回收率为50-150%。其中,抗生素37种,中枢神经系统药物16种,心血管类药物14种,内分泌与计划生育药物12种,抗寄生虫药物8种,非甾体类抗炎药物7种。该方案的检测限和定量限分别为0.001 ~ 11.9 ng L-1和0.003 ~ 39.7 ng L-1。采用该方案对福建省九龙江系列地表水样品进行了上述6类化合物的41种定量鉴定。LODs为1,389 ng L−1(咖啡因)。SPE前的关键步骤是将每个地表水样品的滤液分成两部分,分别调整pH为3和9,并加入0.2 g Na2EDTA。
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