PMID- 29107223 OWN - NLM STAT- MEDLINE DCOM- 20171204 LR - 20171204 IS - 1873-376X (Electronic) IS - 1570-0232 (Linking) VI - 1068-1069 DP - 2017 Nov 15 TI - Rapid gas chromatography with flame photometric detection of multiple organophosphorus pesticides in Salvia miltiorrhizae after ultrasonication assisted one-step extraction. PG - 233-238 LID - S1570-0232(17)31485-X [pii] LID - 10.1016/j.jchromb.2017.10.025 [doi] AB - A simple and rapid gas chromatography-flame photometric detection (GC-FPD) method was developed for the determination of 12 organophosphorus pesticides (OPPs) in Salvia miltiorrhizae by using ultrasonication assisted one-step extraction (USAE) without any clean-up steps. Some crucial parameters such as type of extraction solvent were optimized to improve the method performance for trace analysis. Any clean-up steps were negligent as no interferences were detected in the GC-FPD chromatograms for sensitive detection. Under the optimized conditions, limits of detection (LODs) and quantitation (LOQs) for all pesticides were in the range of 0.001-0.002mg/kg and 0.002-0.01mg/kg and 0.002-0.01mg/kg, respectively, which were all below the regulatory maximum residue limits suggested. RSDs for method precision (intra- and inter-day variations) were lower than 6.8% in approval with international regulations. Average recovery rates for all pesticides at three fortification levels (0.5, 1.0 and 5.0mg/kg) were in the range of 71.2-101.0% with relative standard deviations (RSDs) <13%. The developed method was evaluated for its feasibility in the simultaneous pre-concentration and determination of 12 OPPs in 32 batches of real S. miltiorrhizae samples. Only one pesticide (dimethoate) out of the 12 targets was simultaneously detected in four samples at concentrations of 0.016-0.02mg/kg. Dichlorvos and omethoate were found in the same sample from Sichuan province at 0.004 and 0.027mg/kg, respectively. Malathion and monocrotophos were determined in the other two samples at 0.014 and 0.028mg/kg, respectively. All the positive samples were confirmed by LC-MS/MS. The simple, reliable and rapid USAE-GC-FPD method with many advantages over traditional techniques would be preferred for trace analysis of multiple pesticides in more complex matrices. CI - Copyright (c) 2017 Elsevier B.V. All rights reserved. FAU - Zhang, Shanshan AU - Zhang S AD - Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China; Pharmacy College, Jinzhou Medical University, Jinzhou 121001, China. FAU - Liu, Xiaofei AU - Liu X AD - Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. FAU - Qin, Jia'an AU - Qin J AD - Pharmacy College, Jinzhou Medical University, Jinzhou 121001, China. FAU - Yang, Meihua AU - Yang M AD - Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. FAU - Zhao, Hongzheng AU - Zhao H AD - College of Traditional Chinese Medicine, Jilin Agricultural University, Changchun, 130118, China. FAU - Wang, Yong AU - Wang Y AD - Shimadzu Enterprise Management (China) Limited, Beijing, 100020, China. FAU - Guo, Weiying AU - Guo W AD - Pharmacy College, Jinzhou Medical University, Jinzhou 121001, China. FAU - Ma, Zhijie AU - Ma Z AD - Department of Pharmacy, Beijing Friendship Hospital, Capital Medical University, Beijing 100050, China. Electronic address: 13811647091@163.com. FAU - Kong, Weijun AU - Kong W AD - Key Laboratory of Bioactive Substances and Resources Utilization of Chinese Herbal Medicine, Ministry of Education, Institute of Medicinal Plant Development, Chinese Academy of Medical Sciences & Peking Union Medical College, Beijing 100193, China. Electronic address: kongwj302@126.com. LA - eng PT - Journal Article DEP - 20171014 PL - Netherlands TA - J Chromatogr B Analyt Technol Biomed Life Sci JT - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JID - 101139554 RN - 0 (Organophosphorus Compounds) RN - 0 (Pesticides) SB - IM MH - Chemical Fractionation MH - Chromatography, Gas/*methods MH - Limit of Detection MH - Linear Models MH - Organophosphorus Compounds/*analysis/chemistry/isolation & purification MH - Pesticides/*analysis/chemistry/isolation & purification MH - Reproducibility of Results MH - Salvia miltiorrhiza/*chemistry MH - Sonication/*methods OTO - NOTNLM OT - GC-FPD OT - Multi-residues determination OT - Organophosphorus pesticides OT - Salvia miltiorrhizae OT - Ultrasonication assisted one-step extraction EDAT- 2017/11/07 06:00 MHDA- 2017/12/05 06:00 CRDT- 2017/11/07 06:00 PHST- 2017/08/27 00:00 [received] PHST- 2017/10/12 00:00 [revised] PHST- 2017/10/13 00:00 [accepted] PHST- 2017/11/07 06:00 [pubmed] PHST- 2017/12/05 06:00 [medline] PHST- 2017/11/07 06:00 [entrez] AID - S1570-0232(17)31485-X [pii] AID - 10.1016/j.jchromb.2017.10.025 [doi] PST - ppublish SO - J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 15;1068-1069:233-238. doi: 10.1016/j.jchromb.2017.10.025. Epub 2017 Oct 14.