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Rapid screening of sulfonamides in dietary supplements based on extracted common ion chromatogram and neutral loss scan by LC-Q/TOF-mass spectrometry
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2019-01-01 , DOI: 10.1016/j.jfda.2018.08.006 Nam-Yong Ki 1 , Jisu Hur 1 , Beom Hee Kim 1 , Kyung Ho Kim 2 , Bong Jin Moon 3 , Han Bin Oh 3 , Jongki Hong 1
Journal of Food and Drug Analysis ( IF 2.6 ) Pub Date : 2019-01-01 , DOI: 10.1016/j.jfda.2018.08.006 Nam-Yong Ki 1 , Jisu Hur 1 , Beom Hee Kim 1 , Kyung Ho Kim 2 , Bong Jin Moon 3 , Han Bin Oh 3 , Jongki Hong 1
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There is an increasing amount of dietary supplements that are adulterated with diuretics and anti-diabetic drugs; this has become a global problem due to the wide distribution of dietary supplements and the serious negative health effects of the adulterants. In this study, a rapid screening method was developed for detection and confirmation of 35 sulfonamides in supplements by ultra-high performance liquid chromatography quadrupole/time of flight mass spectrometry. For effective extraction of sulfonamides from dietary supplements, four extraction protocols including HLB and WAX solid-phase extraction, Quick Easy Cheap Effective Rugged and Safe method, and pH-controlled liquid-liquid extraction were evaluated, and pH-controlled liquid-liquid extraction method was shown to be the most effective with high recovery efficiency and low matrix effect. Rapid separation of 35 sulfonamides was achieved with the UHPLC C18 column (150 × 2.1 mm, 1.7 um) within 7 min using ammonium acetate aqueous solution (pH 8) and acetonitrile as the mobile phase. From the MS/MS spectra of sulfonamides, common ions (m/z 77.9650 [SO2N]- and m/z 79.9812 [SO2NH2]-) and neutral molecule loss fragments (HCl and SO2) were observed according to their structural characteristics. Extracted common ion chromatograms and neutral loss scan of these characteristic fragments could effectively apply for rapid screening of sulfonamides in various types of supplements. A reduced mass tolerance window of ±5 ppm was useful for detecting targeted and untargeted sulfonamides and could avoid false positive and false negative results. Overall calibration curves within dynamic range for all targets were shown to be linear with a correlation coefficient R2 > 0.995 and limits of detection ranged from 0.04 to 11.18 ng/g for all sulfonamides. The established method was successfully applied for screening and confirmation of sulfonamides in various supplements. The developed method will be helpful for the identification of sulfonamide diuretics and anti-diabetics in dietary supplements, promoting public health and consumer safety.
中文翻译：
基于提取普通离子色谱和中性丢失扫描的 LC-Q/TOF 质谱快速筛查膳食补充剂中的磺胺类药物
越来越多的膳食补充剂中掺入了利尿剂和抗糖尿病药物；由于膳食补充剂的广泛分布和掺假剂对健康的严重负面影响，这已成为一个全球性问题。本研究开发了一种快速筛选方法，通过超高效液相色谱四极杆/飞行时间质谱法检测和确认补充剂中的 35 种磺胺类药物。对于从膳食补充剂中有效提取磺胺类药物，评估了 HLB 和 WAX 固相萃取、Quick Easy Cheap Effective Rugged and Safe 方法、pH 控制液-液萃取法和 pH 控制液-液萃取法四种提取方案被证明是最有效的，具有高回收率和低基质效应。使用醋酸铵水溶液 (pH 8) 和乙腈作为流动相，使用 UHPLC C18 色谱柱 (150 × 2.1 mm, 1.7 um) 在 7 分钟内实现了 35 种磺胺类药物的快速分离。从磺胺类药物的 MS/MS 谱图中，根据其结构特征观察到常见离子（m/z 77.9650 [SO2N]- 和 m/z 79.9812 [SO2NH2]-）和中性分子丢失碎片（HCl 和 SO2）。这些特征片段的提取常见离子色谱图和中性丢失扫描可有效应用于各类补充剂中磺胺类药物的快速筛选。±5 ppm 的降低质量容差窗口可用于检测靶向和非靶向磺胺类药物，并可避免假阳性和假阴性结果。所有靶标的动态范围内的总体校准曲线均呈线性关系，相关系数 R2 > 0.995，所有磺胺类药物的检测限为 0.04 至 11.18 ng/g。所建立的方法成功地应用于各种补充剂中磺胺类药物的筛选和确认。该方法将有助于鉴别膳食补充剂中的磺胺类利尿剂和抗糖尿病药，促进公众健康和消费者安全。
更新日期：2019-01-01
中文翻译：
基于提取普通离子色谱和中性丢失扫描的 LC-Q/TOF 质谱快速筛查膳食补充剂中的磺胺类药物
越来越多的膳食补充剂中掺入了利尿剂和抗糖尿病药物；由于膳食补充剂的广泛分布和掺假剂对健康的严重负面影响，这已成为一个全球性问题。本研究开发了一种快速筛选方法，通过超高效液相色谱四极杆/飞行时间质谱法检测和确认补充剂中的 35 种磺胺类药物。对于从膳食补充剂中有效提取磺胺类药物，评估了 HLB 和 WAX 固相萃取、Quick Easy Cheap Effective Rugged and Safe 方法、pH 控制液-液萃取法和 pH 控制液-液萃取法四种提取方案被证明是最有效的，具有高回收率和低基质效应。使用醋酸铵水溶液 (pH 8) 和乙腈作为流动相，使用 UHPLC C18 色谱柱 (150 × 2.1 mm, 1.7 um) 在 7 分钟内实现了 35 种磺胺类药物的快速分离。从磺胺类药物的 MS/MS 谱图中，根据其结构特征观察到常见离子（m/z 77.9650 [SO2N]- 和 m/z 79.9812 [SO2NH2]-）和中性分子丢失碎片（HCl 和 SO2）。这些特征片段的提取常见离子色谱图和中性丢失扫描可有效应用于各类补充剂中磺胺类药物的快速筛选。±5 ppm 的降低质量容差窗口可用于检测靶向和非靶向磺胺类药物，并可避免假阳性和假阴性结果。所有靶标的动态范围内的总体校准曲线均呈线性关系，相关系数 R2 > 0.995，所有磺胺类药物的检测限为 0.04 至 11.18 ng/g。所建立的方法成功地应用于各种补充剂中磺胺类药物的筛选和确认。该方法将有助于鉴别膳食补充剂中的磺胺类利尿剂和抗糖尿病药，促进公众健康和消费者安全。
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