{"id":210207,"date":"2020-03-27T18:41:39","date_gmt":"2020-03-27T18:41:39","guid":{"rendered":"https:\/\/docuchem.com\/?page_id=210207"},"modified":"2021-11-22T13:54:50","modified_gmt":"2021-11-22T13:54:50","slug":"hplc-ms-analaysis-of-15-nitrosamines","status":"publish","type":"page","link":"https:\/\/docuchem.com\/en\/hplc-ms-analaysis-of-15-nitrosamines\/","title":{"rendered":"HPLC-MS ANALAYSIS OF 15 NITROSAMINES"},"content":{"rendered":"<p>[et_pb_section fb_built=&#8221;1&#8243; disabled_on=&#8221;off|off|off&#8221; admin_label=&#8221;Header Section&#8221; module_id=&#8221;i-d-analitica&#8221; module_class=&#8221;nosotros-1&#8243; _builder_version=&#8221;4.4.1&#8243; background_color=&#8221;rgba(2,35,40,0.62)&#8221; background_color_gradient_direction=&#8221;360deg&#8221; background_image=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2017\/07\/fondo-estabilidad.jpg&#8221; background_position=&#8221;center_right&#8221; background_blend=&#8221;overlay&#8221; custom_padding=&#8221;0px||0px|&#8221; custom_padding_tablet=&#8221;0px||0px|&#8221; padding_mobile=&#8221;on&#8221; collapsed=&#8221;off&#8221; global_colors_info=&#8221;{}&#8221;][et_pb_row column_padding_mobile=&#8221;on&#8221; custom_padding_last_edited=&#8221;on|desktop&#8221; admin_label=&#8221;row&#8221; _builder_version=&#8221;4.4.1&#8243; background_size=&#8221;initial&#8221; background_position=&#8221;top_left&#8221; background_repeat=&#8221;repeat&#8221; custom_padding=&#8221;5.5%||2.5%|&#8221; custom_padding_tablet=&#8221;&#8221; custom_padding_phone=&#8221;36px||36px|&#8221; global_colors_info=&#8221;{}&#8221;][et_pb_column type=&#8221;4_4&#8243; _builder_version=&#8221;3.25&#8243; background_position=&#8221;top_left&#8221; custom_padding=&#8221;|||&#8221; global_colors_info=&#8221;{}&#8221; custom_padding__hover=&#8221;|||&#8221;][et_pb_text admin_label=&#8221;Preheader&#8221; module_class=&#8221;preheader-int&#8221; _builder_version=&#8221;4.4.1&#8243; text_text_color=&#8221;#c0cd2e&#8221; text_font_size=&#8221;26&#8243; background_size=&#8221;initial&#8221; background_position=&#8221;top_left&#8221; background_repeat=&#8221;repeat&#8221; background_layout=&#8221;dark&#8221; custom_margin=&#8221;||35px|&#8221; text_font_size_tablet=&#8221;16&#8243; text_font_size_phone=&#8221;14&#8243; text_font_size_last_edited=&#8221;on|desktop&#8221; custom_css_main_element=&#8221;font-weight:600;&#8221; border_style=&#8221;solid&#8221; global_colors_info=&#8221;{}&#8221;]<\/p>\n<p>Services<\/p>\n<p>[\/et_pb_text][et_pb_text admin_label=&#8221;T\u00edtulo %22Anal\u00edtica%22&#8243; module_class=&#8221;header-int&#8221; _builder_version=&#8221;4.4.1&#8243; text_font_size=&#8221;62&#8243; header_font_size=&#8221;40px&#8221; background_size=&#8221;initial&#8221; background_position=&#8221;top_left&#8221; background_repeat=&#8221;repeat&#8221; background_layout=&#8221;dark&#8221; max_width_tablet=&#8221;&#8221; max_width_phone=&#8221;&#8221; max_width_last_edited=&#8221;on|phone&#8221; custom_margin=&#8221;||42px|&#8221; text_font_size_tablet=&#8221;35&#8243; text_font_size_phone=&#8221;25&#8243; text_font_size_last_edited=&#8221;on|desktop&#8221; header_font_size_last_edited=&#8221;off|desktop&#8221; custom_css_main_element=&#8221;font-weight:900!important;&#8221; border_style=&#8221;solid&#8221; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h1>HPLC-MS ANALYSIS OF 15 NITROSAMINES <\/h1>\n<p>[\/et_pb_text][\/et_pb_column][\/et_pb_row][\/et_pb_section][et_pb_section fb_built=&#8221;1&#8243; admin_label=&#8221;Our Approach&#8221; module_id=&#8221;nosotros-2&#8243; _builder_version=&#8221;4.4.1&#8243; collapsed=&#8221;off&#8221; global_colors_info=&#8221;{}&#8221;][et_pb_row _builder_version=&#8221;4.4.1&#8243; width=&#8221;90%&#8221; global_colors_info=&#8221;{}&#8221;][et_pb_column type=&#8221;4_4&#8243; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][et_pb_text _builder_version=&#8221;4.4.1&#8243; text_font=&#8221;Cambay||||||||&#8221; text_font_size=&#8221;20px&#8221; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h2>1.1 Introduction<\/h2>\n<p>Docuchem has developed different chromatographic methods using columns with different stationary phases in order to have different possibilities to analyze a broad spectrum of Nitrosamines. In addition, the LOD of 5 Nitrosamines has been tested using a triple quadrupole Shimadzu 8050 MS detector.<\/p>\n<h2>1.2 Scope<\/h2>\n<p>The 15 analyzed Nitrosamines are detailed hereunder:<\/p>\n<ul>\n<li>N-Nitroso-diisobutylamine (NDIBA)<\/li>\n<li>N-Nitroso-dibenzylamine (NDBzA)<\/li>\n<li>N-Nitroso-methylisopropylamine<\/li>\n<li>N-Nitroso-mehtyl aniline (NMA)<\/li>\n<li>N-Nitrosomethylethylamine<\/li>\n<li>N-Nirosodi-n-propylamine (NDPA)<\/li>\n<li>N-Nitrosodi-n-butylamine (NDBA)<\/li>\n<li>N-Nitrosopyrrolidine<\/li>\n<li>N-Nitrosomorpholine<\/li>\n<li>N-Nitroso-N-methyl-4-aminobutyric acid<\/li>\n<li>N-Nitrosoethylisopropylamine (NEIPA)<\/li>\n<li>N-Nitrodiisopropylamine<\/li>\n<li>N-Nitrosodimethylamine<\/li>\n<li>N-Nitrosodiethylamine<\/li>\n<li>N-Nitrosopiperidine (NPIP)<span style=\"color: #505050; font-size: 14px;\">\u00a0<\/span><\/li>\n<\/ul>\n<h2>1.3 HPLC conditions<\/h2>\n<h3>1.3.1\u00a0 Chromatographic conditions with XBridge Phenyl 150&#215;4.6mm 3.5 \u00b5m<\/h3>\n<table width=\"100%\">\n<tbody>\n<tr>\n<td width=\"25%\"><a name=\"_Toc279441285\"><\/a><strong>Column:<\/strong><\/td>\n<td width=\"74%\">XBridge Phenyl 150&#215;4.6mm 3.5 \u00b5m<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Detector:<\/strong><\/td>\n<td width=\"74%\">PDA at 254 nm<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Flow rate:<\/strong><\/td>\n<td width=\"74%\">0.6 mL\/min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Inj. Volume:<\/strong><\/td>\n<td width=\"74%\">5 \u00b5L<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Column oven<\/strong><\/td>\n<td width=\"74%\">40\u00baC<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Run time:<\/strong><\/td>\n<td width=\"74%\">30 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Recording time:<\/strong><\/td>\n<td width=\"74%\">30 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase A:<\/strong><\/td>\n<td width=\"74%\">H<sub>2<\/sub>O 0.1% HCOOH<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase B<\/strong><\/td>\n<td width=\"74%\">Methanol 0.1% HCOOH<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<p><strong>Gradient:<\/strong><\/p>\n<table>\n<tbody>\n<tr>\n<td><strong>Time (minutes)<\/strong><\/td>\n<td><strong>Mobile phase A%<\/strong><\/td>\n<td><strong>Mobile phase B%<\/strong><\/td>\n<\/tr>\n<tr>\n<td>0.00<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>1.5<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>7.0<\/td>\n<td>45<\/td>\n<td>55<\/td>\n<\/tr>\n<tr>\n<td>17.0<\/td>\n<td>45<\/td>\n<td>55<\/td>\n<\/tr>\n<tr>\n<td>17.1<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>21.0<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>21.1<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>25.0<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>30.0<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<h4><\/h4>\n<p>[\/et_pb_text][et_pb_image src=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2020\/03\/1.3.1.1-results-scaled.jpg&#8221; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][\/et_pb_image][et_pb_text _builder_version=&#8221;4.4.1&#8243; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; header_4_font=&#8221;Cambo|700|||||||&#8221; header_4_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h4>1.3.2\u00a0 Chromatographic conditions with Infinitylab Poroshell 120 PFP column<\/h4>\n<p><\/p>\n<table width=\"100%\">\n<tbody>\n<tr>\n<td width=\"25%\"><strong>Column:<\/strong><\/td>\n<td width=\"74%\">Poroshell 120 PFP 100&#215;4.6mm 2.7 \u00b5m<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Detector:<\/strong><\/td>\n<td width=\"74%\">PDA at 254 nm<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Flow rate:<\/strong><\/td>\n<td width=\"74%\">0.6 mL\/min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Inj. Volume:<\/strong><\/td>\n<td width=\"74%\">5 \u00b5L<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Column oven<\/strong><\/td>\n<td width=\"74%\">40\u00baC<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Run time:<\/strong><\/td>\n<td width=\"74%\">30 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Recording time:<\/strong><\/td>\n<td width=\"74%\">30 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase A:<\/strong><\/td>\n<td width=\"74%\">H<sub>2<\/sub>O 0.1% HCOOH<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase B<\/strong><\/td>\n<td width=\"74%\">Methanol 0.1% HCOOH<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Gradient:<\/strong><\/td>\n<td width=\"74%\"><\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<table>\n<tbody>\n<tr>\n<td><strong>Time minutes<\/strong><\/td>\n<td><strong>Mobile phase A%<\/strong><\/td>\n<td><strong>Mobile phase B%<\/strong><\/td>\n<\/tr>\n<tr>\n<td>0.00<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>1.5<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>7.0<\/td>\n<td>45<\/td>\n<td>55<\/td>\n<\/tr>\n<tr>\n<td>17.0<\/td>\n<td>45<\/td>\n<td>55<\/td>\n<\/tr>\n<tr>\n<td>17.1<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>21.0<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>21.1<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>25.0<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<tr>\n<td>30.0<\/td>\n<td>90<\/td>\n<td>10<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<p>[\/et_pb_text][et_pb_image src=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2020\/03\/1.3.2.1-results-scaled.jpg&#8221; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][\/et_pb_image][et_pb_text _builder_version=&#8221;4.4.1&#8243; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; header_4_font=&#8221;Cambo|700|||||||&#8221; header_4_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h4>1.3.4\u00a0 Chromatographic conditions with XSelect CSH Phenyl Hexyl 250X4.6 mm 5 \u00b5m<\/h4>\n<p>&nbsp;<\/p>\n<table width=\"100%\">\n<tbody>\n<tr>\n<td width=\"25%\"><strong>Column:<\/strong><\/td>\n<td width=\"74%\">XSelect CSH Phenyl Hexyl 250&#215;4.6mm 5 \u00b5m<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Detector:<\/strong><\/td>\n<td width=\"74%\">PDA at 254 nm<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Flow rate:<\/strong><\/td>\n<td width=\"74%\">1.0 mL\/min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Inj. Volume:<\/strong><\/td>\n<td width=\"74%\">5 \u00b5L<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Column oven<\/strong><\/td>\n<td width=\"74%\">40\u00baC<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Run time:<\/strong><\/td>\n<td width=\"74%\">32 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Recording time:<\/strong><\/td>\n<td width=\"74%\">32 min<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase A:<\/strong><\/td>\n<td width=\"74%\">H<sub>2<\/sub>O 0.1% HCOOH<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Mobile phase B<\/strong><\/td>\n<td width=\"74%\">Methanol 0.1% HCOOH<\/td>\n<\/tr>\n<tr>\n<td width=\"25%\"><strong>Gradient:<\/strong><\/td>\n<td width=\"74%\">\u00a0<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<table>\n<tbody>\n<tr>\n<td><strong>Time minutes<\/strong><\/td>\n<td><strong>Mobile phase A%<\/strong><\/td>\n<td><strong>Mobile phase B%<\/strong><\/td>\n<\/tr>\n<tr>\n<td>0.0<\/td>\n<td>70<\/td>\n<td>30<\/td>\n<\/tr>\n<tr>\n<td>10.0<\/td>\n<td>50<\/td>\n<td>50<\/td>\n<\/tr>\n<tr>\n<td>14.0<\/td>\n<td>50<\/td>\n<td>50<\/td>\n<\/tr>\n<tr>\n<td>21.0<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>25.0<\/td>\n<td>10<\/td>\n<td>90<\/td>\n<\/tr>\n<tr>\n<td>25.1<\/td>\n<td>70<\/td>\n<td>30<\/td>\n<\/tr>\n<tr>\n<td>32.0<\/td>\n<td>70<\/td>\n<td>30<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<h4><\/h4>\n<p>[\/et_pb_text][et_pb_image src=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2020\/03\/1.3.4.1-results-scaled.jpg&#8221; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][\/et_pb_image][et_pb_text _builder_version=&#8221;4.4.1&#8243; text_font=&#8221;Cambay||||||||&#8221; text_font_size=&#8221;20px&#8221; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; header_4_font=&#8221;Cambo|700|||||||&#8221; header_4_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h2>1.4 Limit of Detection of Nitrosamines<\/h2>\n<p>The LOD of 5 different Nitrosamines: (N-Nitroso-Dimethylamine (NDMA), N-Nitroso-Piperidine (NPID), N-Nitroso-Diethylamine (NDEA), N-Nitroso-Ethylisopropylamine (NEIPA) and N-Nitroso-Diisopropylamine (NDIPA) has been evaluated with a triple quadrupole MS detector 8050 from Shimadzu using the HPLC method conditions with the XBridge C18 column.<\/p>\n<p>[\/et_pb_text][et_pb_image src=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2020\/03\/grafic1.jpg&#8221; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][\/et_pb_image][et_pb_text _builder_version=&#8221;4.4.1&#8243; text_font=&#8221;Cambay||||||||&#8221; text_font_size=&#8221;20px&#8221; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; header_4_font=&#8221;Cambo|700|||||||&#8221; header_4_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<p><span>Combining the HPLC methods developed by Docuchem and optimizing the MS\/MS conditions, LOD of 2.5 ppb can be achieved for the 5 tested Nitrosamines. For NPID, NEIPA and NDIPA, the LOD could be lowered even more, reaching levels below 1 ppb.<\/span><\/p>\n<p><span>Further investigations were performed obtaining a LOD of 0.1 ppb for NDMA using an UPLC method. <\/span><\/p>\n<p>[\/et_pb_text][et_pb_image src=&#8221;https:\/\/docuchem.com\/wp-content\/uploads\/2020\/03\/grafic2.jpg&#8221; _builder_version=&#8221;4.4.1&#8243; global_colors_info=&#8221;{}&#8221;][\/et_pb_image][et_pb_text _builder_version=&#8221;4.4.1&#8243; text_font=&#8221;Cambay||||||||&#8221; text_font_size=&#8221;20px&#8221; header_2_font=&#8221;Cambo||||||||&#8221; header_2_text_color=&#8221;#5F7EB9&#8243; header_4_font=&#8221;Cambo|700|||||||&#8221; header_4_text_color=&#8221;#5F7EB9&#8243; global_colors_info=&#8221;{}&#8221;]<\/p>\n<h2>1.5 Conclusions<\/h2>\n<p>The different HPLC methods tested provides flexibility in the HPLC separation. Depending on the Nitrosamines that the costumer needs to analyze and the other substances contained in the sample, the previously listed HPLC methods can be used to achieve suitable resolutions between the analytes. For NDMA, a LOD of 0.1ppb was achieved after an optimization of the MS parameters. Therefore, LOD of all nitrosamines could be improved obtaining LOD results about 0.5ppb or even lower<\/p>\n<p>[\/et_pb_text][\/et_pb_column][\/et_pb_row][\/et_pb_section]<\/p>\n","protected":false},"excerpt":{"rendered":"<p>ServicesHPLC-MS ANALYSIS OF 15 NITROSAMINES 1.1 Introduction Docuchem has developed different chromatographic methods using columns with different stationary phases in order to have different possibilities to analyze a broad spectrum of Nitrosamines. In addition, the LOD of 5 Nitrosamines has been tested using a triple quadrupole Shimadzu 8050 MS detector. 1.2 Scope The 15 analyzed [&hellip;]<\/p>\n","protected":false},"author":56,"featured_media":0,"parent":0,"menu_order":0,"comment_status":"closed","ping_status":"closed","template":"","meta":{"_et_pb_use_builder":"on","_et_pb_old_content":"","_et_gb_content_width":"","footnotes":""},"yoast_head":"<!-- This site is optimized with the Yoast SEO plugin v21.8 - https:\/\/yoast.com\/wordpress\/plugins\/seo\/ -->\n<title>HPLC-MS ANALAYSIS OF 15 NITROSAMINES - Docuchem | Espa\u00f1a<\/title>\n<meta name=\"robots\" content=\"index, follow, max-snippet:-1, max-image-preview:large, max-video-preview:-1\" \/>\n<link rel=\"canonical\" href=\"https:\/\/docuchem.com\/en\/hplc-ms-analaysis-of-15-nitrosamines\/\" \/>\n<meta property=\"og:locale\" content=\"en_US\" \/>\n<meta property=\"og:type\" content=\"article\" \/>\n<meta property=\"og:title\" content=\"HPLC-MS ANALAYSIS OF 15 NITROSAMINES - Docuchem | Espa\u00f1a\" \/>\n<meta property=\"og:description\" content=\"ServicesHPLC-MS ANALYSIS OF 15 NITROSAMINES 1.1 Introduction Docuchem has developed different chromatographic methods using columns with different stationary phases in order to have different possibilities to analyze a broad spectrum of Nitrosamines. 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