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Evaluation of selected pharmaceuticals and personal care products in water matrix using ion trap mass spectrometry: A simple weighted calibration curve approach.
Journal of Pharmaceutical and Biomedical Analysis ( IF 3.1 ) Pub Date : 2020-02-26 , DOI: 10.1016/j.jpba.2020.113214
Chikmagalur Mallappa Gopal 1 , Krishnamurthy Bhat 2 , Yerabham Praveenkumarreddy 1 , Shailesh 3 , Virendra Kumar 4 , Hirakendu Basu 5 , Derrick Ian Joshua 6 , Rakesh Kumar Singhal 5 , Keshava Balakrishna 1
Affiliation  

A novel analytical method is presented for 12 target pharmaceutical and personal care products (PPCPs), belonging to different classes like antibiotics, non-steroid anti-inflammatory drugs, parabens, UV-filters, plasticizer, and antibacterials. The method development comprises of solid-phase extraction (SPE) with lipophilic-hydrophilic material balanced Oasis HLB cartridge, followed by reverse-phase liquid chromatography interfaced to linear ion trap tandem mass spectrometry (LC-MS/MS) with electrospray ionization. Chromatographic separation was achieved with a gradient elution of 25 min run time using 5 mM ammonium acetate buffer with pH adjustment using acetic acid. In addition, cost effective organic solvent with buffer used together as the mobile phase with Chromatopak C18 column (150 mm × 4 mm, 5-μm,) in negative ionization mode. Recoveries ranged from 61.74 % to 119.89 % for most of the compounds. Matrix-matched calibration curves were used for counterbalancing the matrix effects for all the analytes, and ibuprofen D3 internal standard was used for assessing the effectiveness of extraction technique and monitoring the recovery of sample analysis. Simple empirical weighted linear regression curve technique was adopted practically for each analysis in enhancing the analyte accuracy at lower quantification level. The 1/x2 model was selected as the best suitable model for quantification of analytes, which can be evaluated by deviation from back-calculated concentration in terms of percentage relative error (%RE). Weighted calibration curves with regression value for most of the compounds were ≥ 0.98, except triclosan with a regression value ≥ 0.93. Precision showed as % relative standard deviation (%RSD) were always below 15.0 %. Accuracy-test was evaluated by the statistical one-sample t-test and no significant difference was observed between nominal and experimental value. The limit of quantification (LOQ) ranged from 3.0 ng/mL (BP1) to 1000 ng/mL (naproxen). Finally, the validated method was used for the first time to determine target analytes in surface water samples collected from Arkavathi river flowing across southern India's Bengaluru city.

中文翻译:

使用离子阱质谱法评估水基质中的选定药物和个人护理产品:一种简单的加权校准曲线方法。

提出了一种针对12种目标药物和个人护理产品(PPCP)的新颖分析方法,这些产品属于不同类别,例如抗生素,非甾体抗炎药,对羟基苯甲酸酯,紫外线过滤剂,增塑剂和抗菌剂。该方法的开发包括:使用亲脂-亲水材料平衡的Oasis HLB柱进行固相萃取(SPE),然后通过电喷雾电离与线性离子阱串联质谱法(LC-MS / MS)进行反相液相色谱分析。使用5 mM醋酸铵缓冲液(运行时间为25分钟)进行梯度洗脱,并使用乙酸调节pH,从而实现色谱分离。此外,具有成本效益的有机溶剂与缓冲液一起在Chromatopak C18色谱柱(150 mm×4 mm,5-μm)中以负电离模式一起用作流动相。大多数化合物的回收率在61.74%至119.89%之间。基质匹配的校准曲线用于平衡所有分析物的基质效应,布洛芬D3内标用于评估萃取技术的有效性并监测样品分析的回收率。对于每个分析,实际上都采用简单的经验加权线性回归曲线技术,以提高较低定量水平的分析物准确性。选择1 / x2模型作为最适合分析物定量的模型,可以通过相对于百分比的相对误差(%RE)与反算浓度的偏差进行评估。除三氯生的回归值≥0.93外,大多数化合物的回归值加权校正曲线均≥0.98。精度显示为相对标准偏差百分比(%RSD)始终低于15.0%。准确性测试是通过统计的一样本t检验进行评估的,在标称值和实验值之间未观察到显着差异。定量限(LOQ)为3.0 ng / mL(BP1)至1000 ng / mL(萘普生)。最后,经过验证的方法首次用于测定从流经印度南部班加罗尔市的Arkavathi河收集的地表水样品中的目标分析物。
更新日期:2020-02-26
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