色谱最新文献

{"title":"超高效液相色谱-四极杆-飞行时间质谱法快速筛查和确证渔药中86种非法添加化学品","authors":"Qingqing Ke, Shiyan Li, Dingnan Wang, Qin Zhou, Fan Zhou, Yijiang Bei, Xiaoming Chen, Yang Wang","doi":"10.3724/SP.J.1123.2021.11023","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.11023","url":null,"abstract":"建立了超高效液相色谱-四极杆-飞行时间质谱法快速筛查与确证渔药中86种非法添加禁限用药物的方法。渔药以80%(v/v)乙腈水溶液进行提取,通过稀释降低基质效应,采用ACQUITY PREMIER HSS T3色谱柱进行分离,以甲醇和0.1%甲酸水溶液作为流动相进行梯度洗脱,采用电喷雾双喷离子源(Dual AJS ESI)正离子模式分析检测。建立了86种药物的一级精确质量数据库和二级碎片质谱库。在全扫描采集模式下,以化合物的色谱保留时间、精确质量数、同位素分布和同位素丰度比定性;在Target MS/MS采集模式下,通过二级碎片离子的匹配进一步确证化合物,以准分子离子峰的峰面积定量,实现渔药样品中多目标药物的快速定性定量分析。86种药物在各自的线性范围内均呈现良好的线性关系,相关系数均大于0.99,中草药制剂和抗生素粉剂的定量限(LOQ)范围分别为1~15 mg/kg和5~75 mg/kg,添加回收率范围为76.8%~112.1%,相对标准偏差(RSD, n=3)小于11.7%。该方法快速、简便、准确、灵敏,适用于不同种类渔药中禁限用非法添加药物的高通量筛查。将该方法应用于浙江省渔用投入品质量安全监督抽检项目中,共筛查60个样品,其中8种中草药制剂筛查出说明书中未明确标明的药物成分,1种抗生素粉剂未检出有效成分。该研究为渔药的质量安全监控提供了有效的技术手段。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"520 - 530"},"PeriodicalIF":0.7,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41569017","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"气相色谱-负化学源质谱法测定船舶压载水中4种三卤甲烷","authors":"Guoshen Hu, Hong Wang, Ke-yao Yu, Wei-jian Shen, Y. Hou, Meiquan Ji, Yiming Zhu, W. Tian, Xidong Li","doi":"10.3724/SP.J.1123.2022.01003","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.01003","url":null,"abstract":"我国每年的船舶压载水排放量巨大,压载水中含有浮游生物、病原体及其幼虫或孢子等,若处理不当,会对排放水域的生态环境造成严重影响。排放压载水前常使用电解法对其进行处理,电解产生的次氯酸钠溶液,能有效杀灭残余的微生物。但电解后会产生副产物三卤甲烷(THMs),其对人体有一定的健康风险,建立船舶压载水中三卤甲烷的测定方法具有重要意义。该研究建立了采用气相色谱-负化学源质谱(GC-NCI-MS)测定船舶压载水中4种三卤甲烷(包括三氯甲烷、二氯一溴甲烷、一氯二溴甲烷、三溴甲烷)的分析方法。船舶压载水样品经过顶空进样技术处理后,通过DB-5MS UI毛细管色谱柱(30 m×0.25 mm×1.0 μm)分离,气相色谱-负化学源质谱仪测定,在选择离子扫描(SIM)模式下分析,采用外标法进行定量。4种三卤甲烷在0.2~50 μg/L范围内线性关系良好,相关系数(r)≥0.995,定量限(S/N=10)为0.1~0.2 μg/L,在0.2、0.5、2.0 μg/L 3个加标水平下,4种THMs的平均回收率为90.3%~106.8%,相对标准偏差(RSD)为1.4%~6.2%。该方法准确、稳定、可靠,可用于测定船舶压载水中4种THMs的含量。使用建立的测定方法对36个船舶压载水进行测定,三溴甲烷、二溴一氯甲烷、一溴二氯甲烷与三氯甲烷的检出率分别为83.3%、69.4%、22.2%和19.4%,检出值分别为34.25~221.5 μg/L、3.52~41.87 μg/L、1.52~8.56 μg/L和0.02~5.46 μg/L。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"584 - 589"},"PeriodicalIF":0.7,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46822312","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"基于液相色谱-串联质谱的结肠癌血清氧固醇标志物筛选","authors":"Zhanjun Ma, Zheng Li, Huan Wang, Ren-Hua Wang, Xiaofei Han","doi":"10.3724/SP.J.1123.2022.01001","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2022.01001","url":null,"abstract":"结肠癌(CC)是全球常见恶性肿瘤之一,发病率呈逐年上升趋势,目前没有有效的标志物用于疾病早期诊断和干预跟踪。胆固醇及其氧化衍生物氧固醇在众多恶性肿瘤发生发展中发挥关键作用。该研究采用液相色谱-串联质谱(LC-MS/MS)技术,对CC临床血清样本中胆固醇及相关10种氧固醇代谢物进行了定性定量分析,并采用偏最小二乘判别分析(PLS-DA)和正交偏最小二乘判别分析(OPLS-DA)进行多元统计分析,发现上述目标代谢物能够较好地区分CC组与健康对照组。为防止数据过拟合,该研究在PLS-DA模型各代谢物变量投影重要性(VIP)基础上,结合最优组分数及K-均值聚类结果,筛选得到3种代谢标志物。通过受试者操作特征曲线(ROC)的曲线下面积(AUC)分析,发现筛选得到的3种潜在标志物联合预测CC达到0.998,说明模型性能优良。GO(基因本体论)富集分析显示3种潜在标志物主要分布在内质网和包被囊泡上,参与胆固醇代谢、运输、低密度脂蛋白重塑等生物进程,发挥胆固醇运输活性和低密度脂蛋白颗粒受体结合的分子功能。KEGG(京都基因与基因组百科全书)通路分析显示3种潜在标志物富集于类固醇生物合成、PPAR(过氧化物酶体增殖物激活受体)信号通路及ABC(ATP结合盒)转运等通路上。该研究为寻找CC标志物及进一步阐明胆固醇及氧固醇在CC发病过程中的作用奠定了一定的基础。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"541 - 546"},"PeriodicalIF":0.7,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44500370","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Rapid screening of 84 pesticide residues in dendrobium by Sin-QuEChERS Nano purification column with gas chromatography-tandem mass spectrometry].","authors":"Quan Zhang, Shan Bi, Yutian Wu, Lei Li, Yibing Zhou, Liya Liu, Wenzheng Liu, Qingyuan Chen, Xue Zhou, Hua Guo","doi":"10.3724/SP.J.1123.2021.12010","DOIUrl":"10.3724/SP.J.1123.2021.12010","url":null,"abstract":"<p><p>A rapid screening method for 84 pesticide residues in dendrobium perfringens parent material with different polarities was developed using a Sin-QuEChERS Nano clean-up column combined with gas chromatography-tandem mass spectrometry (GC-MS/MS). The differences in extraction efficiency of the targets were compared with different extraction solvents (acetonitrile containing 1% acetic acid, acetone) and methods (immersion with or without water). The purification effect and extraction recoveries of Sin-QuEChERS Nano method and classical dispersive solid-phase extraction (dSPE), solid-phase extraction (SPE) and QuEChERS were systematically compared using <i>Dendrobium nobile</i> samples. The differences in matrix effects between the Sin-QuEChERS Nano method, which was more effective in purification, and the dSPE method were also analyzed. The purification effects of three commercially available Sin-QuEChERS Nano purification columns (simple matrix purification column, complex matrix purification column and herbal purification column) were compared. The applicability of the purification methods were also verified by using different parts of <i>Dendrobium nobile</i> samples (stems, leaves and flowers). From the results, it could be concluded that weighing 2.00 g and the samples in 5 mL of water for 20 min, followed by extraction with acetonitrile containing 1% acetic acid was more effective. The average extraction recovery of the target components by Sin-QuEChERS Nano purification method was 90.5%, which further identified Sin-QuEChERS Nano-Chinese medicine purification column as the preferred purification column for dendrobium purification. The target components were separated by a DB-1701MS quartz capillary column (30 m×0.25 mm×0.25 μm) with programmed temperature rise, detected by multiple reaction monitoring (MRM) mode, and quantified by matrix-matched solution external standard method. The GC-MS/MS assay was used for the methodological validation of the 84 representative pesticides within <i>Dendrobium officinale</i> and <i>Dendrobium nobile</i> was carried out by GC-MS/MS detection method. The results indicated that the targets showed excellent linear correlation in different scopes with correlation coefficients (<i>r</i><sup>2</sup>) >0. 990. The limits of detection (LODs, <i>S/N</i>=3) of the method were 1.5 to 5.8 μg/kg, and the limits of quantification (LOQs, <i>S/N</i>=10) ranged from 5.0 to 15.0 μg/kg. The spiked recoveries of the target pesticides under different spiked levels were 68.7%-116.2%, and the relative standard deviations (RSDs, <i>n</i>=6) were less than 15%. Compared to other typical pretreatment methods, the Sin-QuEChERS Nano method provided better performance in terms of purification. The method not only effectively removed pigments, organic acids, and alkaline interferents, but also saved preparation time. Losses due to solvent transfer were also avoided and no further vortexing or centrifugation was required, making it","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"565-575"},"PeriodicalIF":1.2,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404037/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43881727","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"[Highly sensitive determination of three kinds of amanitins in urine and plasma by ultra performance liquid chromatography-triple quadrupole mass spectrometry coupled with immunoaffinity column clean-up].","authors":"Xiuyao Zhang, Xinxin Cai, Xiaoyi Zhang, Ruifen Li, Yunfeng Zhao","doi":"10.3724/SP.J.1123.2021.08018","DOIUrl":"10.3724/SP.J.1123.2021.08018","url":null,"abstract":"<p><p>Cases of toxic mushroom poisoning occur frequently in China every year. In particular, mushrooms containing amanitins can cause acute liver damage, with high mortality rates. The symptoms of acute liver damage are experienced 9-72 h after consumption of the mushrooms. At this time, the concentration of amanitins in blood and urine is too low to be detected even by the highly sensitive ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS), thus rendering clinical diagnosis and treatment difficult. To this end, a method was developed for the determination of <i>α</i>-amanitin, <i>β</i>-amanitin and <i>γ</i>-amanitin in urine and plasma by UPLC-MS/MS. Urine and plasma samples were extracted and cleaned up by using an immunoaffinity column. A sample of 2.00 mL urine or 1.00 mL of plasma was diluted with 8.00 mL of phosphate buffer solution (PBS) and then loaded onto the immunoaffinity column at a flow rate of 0.5-1.0 mL/min. After washing the column with 10 mL of PBS and 13 mL of water successively, the bound amanitins were eluted with 3.00 mL of methanol-acetone (1∶1, v/v). The eluent was dried under nitrogen at 55 ℃. The residue was dissolved in 100 μL of 10% (v/v) methanol aqueous solution. The amanitins in urine were concentrated 20 times, while those in plasma were concentrated 10 times. Chromatographic separation was performed on a Kinetex Biphenyl column (100 mm × 2.1 mm, 1.7 μm) with gradient elution using methanol and 0.005% (v/v) formic acid aqueous solution as mobile phases. The three amanitins were detected by negative electrospray ionization tandem mass spectrometry in the multiple reaction monitoring (MRM) mode and quantified by the solvent standard curve external standard method. Method validation was performed as recommended by the European Drug Administration (EMEA). Four levels of quality control (QC) samples were prepared, which covered the calibration curve range, viz., the limit of quantification (LOQ), within three times the LOQ (low QC), medium QC, and at 85% of the upper calibration curve range (high QC), and used to test the accuracy, precision, matrix effect, extraction recovery, and stability. The calibration curves for the three amanitins showed good linear relationships in the range of 0.1-200 ng/mL, and the correlation coefficients (<i>r</i>) were greater than 0.999. The matrix effects and extraction efficiencies of the three amanitins in urine and plasma were 92%-108% and 90%-103%, respectively, and the coefficients of variation were less than 13%. The accuracies of the three amanitins in urine were within -9.4%-8.0%. The repeatability and intermediate accuracies were 3.0%-14% and 3.5%-18%, respectively. When the sampling volume was 2.00 mL, the limits of detection of the three amanitins in urine were 0.002 ng/mL. The accuracies of the three amanitins in plasma were within -13%-8.0%. The repeatability and intermediate accuracies were 3.9%-9.7% and 5.5%-12%, respectively. When the","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"443-451"},"PeriodicalIF":1.2,"publicationDate":"2022-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404148/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"69765278","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"固相萃取-气相色谱-串联质谱法同时测定武汉市普通人群血清中35种有机氯农药与多氯联苯","authors":"Xiang Li, Limei Wang, Lulu Song, Zhengce Wan, Jing Kou, M. Zhang, Yongman Lü, Youjie Wang, Surong Mei","doi":"10.3724/SP.J.1123.2021.12013","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.12013","url":null,"abstract":"有机氯农药(OCPs)和多氯联苯(PCBs)是两类重要的持久性有机污染物,可在环境介质中长期存在,并通过多种途径进入人体,导致人体的高暴露风险。OCPs和PCBs对人体存在诸多健康危害,精准定量人体内OCPs和PCBs的暴露水平是健康效应评价的关键。该研究基于固相萃取-气相色谱-串联质谱联用技术(SPE-GC-MS/MS)建立了同时检测100 μL血清中35种OCPs和PCBs的分析方法。血清样品经尿素沉淀蛋白后,采用Oasis® HLB小柱净化,正己烷-二氯甲烷混合溶液(1∶1, v/v)洗脱,氮吹近干,正己烷定容,多反应监测(MRM)模式检测,内标法定量分析。结果表明,OCPs和PCBs在0.05~50.0 ng/mL范围内线性关系良好,检出限在1.2~71.4 ng/L之间。35种目标分析物的加标回收率在72.6%~142%之间,相对标准偏差小于25%。利用所建立的方法检测了武汉市普通人群血清样本中OCPs和PCBs的浓度水平,结果表明武汉市普通人群广泛暴露于OCPs和PCBs,且以OCPs为主。有8种OCPs和7种PCBs检出率高于50%,其中p,p'-滴滴伊、p,p'-滴滴滴和甲氧滴滴涕检出率达100%,非类二噁英PCBs是PCBs的主要成分。血清中OCPs浓度随年龄增长呈升高趋势,在60岁以上存在性别差异;不同性别、年龄人群血清中PCBs浓度无统计学差异。该方法样本用量少,操作简便,具有较高的准确度和精密度,适用于环境健康研究中大量人群血清样本中痕量OCPs和PCBs的生物监测。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"191 1","pages":"461 - 468"},"PeriodicalIF":0.7,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88484060","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"QuEChERS-气相色谱-质谱法检测鱼肉中19种氯酚类化合物","authors":"Yinghua Mu, Jiali Xing, Jian Shen, Lu Ying, Lingyan Mao, Xiaorong Xu, Yongjiang Lou, Xi Wu","doi":"10.3724/SP.J.1123.2021.12002","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.12002","url":null,"abstract":"大量含氯农药、次氯酸消毒水以及水产品杀虫剂和杀菌剂的广泛使用,使鱼类容易受到氯酚类化合物的污染,因而建立鱼肉中氯酚类化合物的检测方法十分重要。建立了QuEChERS结合气相色谱-质谱法同时检测鱼肉中19种氯酚类化合物的分析方法。19种氯酚类化合物选用DB-5MS毛细管色谱柱(30 m×0.25 mm×0.25 μm),载气流速1 mL/min进行分离,可以得到很好的峰形。前处理采用改良的QuEChERS方法,通过对提取剂的种类和剂量、净化剂的种类和剂量,以及衍生条件中的衍生温度、衍生时间和衍生剂用量等进行优化,确定最优的前处理方法。选择10 mL乙酸乙酯作为提取剂,500 mg的C18作为净化剂,加入3 g氯化钠和5 g无水硫酸镁,过0.22 μm的有机滤膜,加入50 μL的硅烷化衍生剂在45 ℃条件下衍生30 min,用EI源测定,选择离子监测模式,以外标法定量。19种氯酚类化合物在0.4~10 μg/L范围内具有良好的线性关系,相关系数R2大于0.998,方法定量限为0.04~0.16 μg/kg。空白基质不同加标水平的回收率为70.6%~115.0%,相对标准偏差为2.6%~10.5%。将建立的方法应用于实际样品的检测分析,结果显示,各种鱼肉中均有不同程度的氯酚类化合物检出,其中,黄花鱼检出的氯酚类化合物总量最大,为8.74 μg/kg;其次为鲫鱼7.59 μg/kg;米鱼的检出量最少,为1.59 μg/kg。所建立的方法简化了样品的前处理步骤,操作简单,方法灵敏度高、重复性好,可满足鱼肉中19种氯酚类化合物的高通量检测要求,能显著提高氯酚类化合物的检测效率。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"35 1","pages":"477 - 487"},"PeriodicalIF":0.7,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75080629","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"固相萃取-高效液相色谱-串联质谱法同时测定燕窝中45种激素及其水平调查","authors":"Dunming Xu, Sanmei Zeng, Xuncai Liu, Luxiao Wang, Qunyan Fan, Xiaojiang Zhang, Enhua Fang","doi":"10.3724/SP.J.1123.2021.08008","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.08008","url":null,"abstract":"建立了固相萃取-高效液相色谱-串联质谱(SPE-HPLC-MS/MS)同时测定食用燕窝中皮质激素、雌激素、雄激素及孕激素等5类45种激素的多残留分析方法。采用乙腈-乙酸乙酯(1∶1, v/v)超声辅助提取、亲水亲脂平衡固相萃取柱净化,甲醇洗脱。分别在正、负电喷雾电离源、多反应监测模式下检测45种激素。正离子模式下的流动相为乙腈-0.1%甲酸水溶液,负离子模式下的流动相为乙腈-水,色谱柱为Phenomenex Kinetex C18柱(100 mm×2.1 mm, 2.6 μm)。在优化条件下,45种激素在0.20~20.0 μg/L范围内线性关系良好,相关系数(R2)≥0.9990,方法的检出限(LOD)为0.04~0.70 μg/kg,定量限(LOQ)为0.16~2.00 μg/kg。按三水平(2.0、4.0、20.0 μg/kg)进行加标回收试验,氟米龙、布地奈德、醛固酮、醋酸氟轻松、炔雌醇的回收率为40.2%~63.6%,可对这5种激素进行定性分析,其余40种激素的平均加标回收率为72.2%~112.3%,相对标准偏差(RSD)为2.5%~11.6%,该方法可对40种激素进行准确定性定量,精密度好,灵敏度高,简便、快速。从2017~2021年,通过研究建立的方法对来自马来西亚、印度尼西亚、泰国和越南等国家的1021个燕窝样品进行监测,仅勃地酮、雄烯二酮、孕酮有检出(大于检出限),其他激素均小于检出限。孕酮检出率为100%,勃地酮、雄烯二酮检出率分别为79%和89%, 3种激素含量范围分别为0.097~3.58、0~0.096和0~1.77 μg/kg。与同为动物源性食品的鸡蛋、纯牛奶、乳制品相比,所有测定的鸡蛋样品中均检出雄烯二酮,含量比其他3类产品略高;勃地酮在4类产品中的含量差别不大,均为微量;孕酮含量在鸡蛋中最高,其次是纯牛奶,燕窝中含量最低。研究结果表明,食用燕窝带入的激素种类少,含量低,对健康影响小。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"423 - 432"},"PeriodicalIF":0.7,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"69765270","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"超高效液相色谱-四极杆-飞行时间高分辨质谱快速筛查确证化妆品中73种常见禁用物质","authors":"Yang-Shyang Li, Jiaying Huang, Jihui Fang, Zhiqiang Huang","doi":"10.3724/SP.J.1123.2021.09010","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.09010","url":null,"abstract":"建立了超高效液相色谱-四极杆-飞行时间高分辨质谱(UPLC-Q-TOF HRMS)同时快速筛查确证化妆品中73种常见禁用物质的方法。样品经饱和氯化钠溶液分散均匀后,采用含0.2%甲酸的乙腈溶液超声提取,50 mg PSA净化,以8000 r/min高速冷冻离心除脂,采用Waters Acquity HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm)分离。采用多反应监测高分辨扫描模式(MRM HR),以保留时间、一级母离子精确质量数、同位素丰度比和二级子离子精确质量数实现化妆品中73种禁用物质的快速筛查和确证,基质匹配外标法定量。实验比较了不同提取溶剂、净化吸附剂、色谱条件和质谱扫描模式对73种禁用物质测定的影响,并考察了膏霜剂和水剂的基质效应。结果表明,73种禁用物质线性关系良好,相关系数(R2)>0.99;检出限为5~150 μg/kg;定量限为15~450 μg/kg;膏霜剂及水剂两种基质在3个加标水平下的回收率为60.3%~130.3%,日内、日间RSD分别为0.8%~10.0%(n=6)和1.1%~15.0%(n=3)。日常风险监测中检出磺胺甲基异噁唑、甲基泼尼松、林可霉素、对乙酰氨基酚、甲氧苄啶、阿法骨化醇、倍他米松戊酸酯、溴莫尼定、氯霉素、氯苯那敏、氯倍他索丙酸酯、克罗米通、益康唑、酮康唑、泼尼松醋酸酯和泼尼松,检出含量范围为0.5~1136.1 mg/kg。该方法准确、快速、简便,可用于化妆品中73种常见禁用物质的检测。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"433 - 442"},"PeriodicalIF":0.7,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"69765347","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"加速溶剂提取-同位素稀释-高分辨气相色谱-高分辨质谱法测定生物样品中82种多氯联苯","authors":"Yinju Wu, Bailu Qu, Y. Hou, Haibin Yu, Renji Xu, Xiaoyan Zheng","doi":"10.3724/SP.J.1123.2021.10018","DOIUrl":"https://doi.org/10.3724/SP.J.1123.2021.10018","url":null,"abstract":"我国水产品中多氯联苯(PCBs)的检测方法,主要以6种指示性PCBs和12种二噁英类共平面PCBs为主,仅涵盖有限的PCBs。为更全面地获得生物体中PCBs的浓度水平,深入探讨PCBs在生物体内的代谢和富集特征,进而准确评价PCBs对人类的暴露水平及风险,以鱼和贝类作为生物样品代表,建立了加速溶剂提取-同位素稀释-高分辨气相色谱-高分辨质谱(ASE-ID-HRGC-HRMS)测定生物样品中82种PCBs的方法。比较了振荡提取和加速溶剂提取两种提取方式的回收率和重复性,最终采用正己烷-二氯甲烷(1∶1, v/v)对PCBs进行加速溶剂提取。考察了各流分淋洗液对PCBs的回收率,确定了样品提取液经8 g 44%酸性硅胶层析柱(内径15 mm), 90 mL正己烷洗脱的净化方式。样品提取液净化浓缩后进行HRGC-HRMS分析,色谱柱采用DB-5MS超低流失石英毛细管柱(60 m×0.25 mm×0.25 μm)。通过优化后的升温程序对化合物进行分离,以保留时间和两个特征离子精准定性,采用同位素内标法定量。结果表明,在0.1~200 μg/L范围内,平均相对响应因子(RRF)的相对标准偏差值(RSD, n=7)均≤20%,相关系数(r2)>0.99。生物样品中PCBs的方法检出限为0.02~3 pg/g;鱼类中PCBs平均加标回收率为71.3%~141%, RSD(n=7)为2.1%~14%;贝类中PCBs平均加标回收率为76.9%~143%, RSD为1.4%~11%。该方法灵敏、准确、可靠,可以更加全面具体地分析鱼和贝类等水产品受PCBs的污染情况,为国内外开展生物监测提供有效的技术支持,从而服务于相关生态环境管理及履行《斯德哥尔摩公约》。","PeriodicalId":9864,"journal":{"name":"色谱","volume":"40 1","pages":"452 - 460"},"PeriodicalIF":0.7,"publicationDate":"2022-05-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47983792","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}