ГОСТ 34480-2018 Мясо и мясные продукты. Определение амфениколов и пенициллинов методом тандемной жидкостной масс-спектрометрии
ГОСТ 34480-2018
МЕЖГОСУДАРСТВЕННЫЙ СТАНДАРТ
МЯСО И МЯСНЫЕ ПРОДУКТЫ
Определение амфениколов и пенициллинов методом тандемной жидкостной масс-спектрометрии
Meat and meat products. Determination of amphenicols and penicillins by tandem liquid mass spectrometry method
МКС 67.120.10
Дата введения 2019-10-01
Предисловие
Цели, основные принципы и основной порядок проведения работ по межгосударственной стандартизации установлены в ГОСТ 1.0-2015 "Межгосударственная система стандартизации. Основные положения" и ГОСТ 1.2-2015 "Межгосударственная система стандартизации. Стандарты межгосударственные, правила и рекомендации по межгосударственной стандартизации. Правила разработки, принятия, обновления и отмены"
Сведения о стандарте
1 РАЗРАБОТАН Федеральным государственным бюджетным научным учреждением "Федеральный научный центр пищевых систем им.В.М.Горбатова" РАН (ФГБНУ "ФНЦ пищевых систем им.В.М.Горбатова" РАН)
2 ВНЕСЕН Федеральным агентством по техническому регулированию и метрологии
3 ПРИНЯТ Межгосударственным советом по стандартизации, метрологии и сертификации (протокол от 30 октября 2018 г. N 113-П)
За принятие проголосовали:
Краткое наименование страны |
Код страны |
Сокращенное наименование национального органа по стандартизации |
Армения |
AM |
Минэкономики Республики Армения |
Беларусь |
BY |
Госстандарт Республики Беларусь |
Казахстан |
KZ |
Госстандарт Республики Казахстан |
Киргизия |
KG |
Кыргызстандарт |
Россия |
RU |
Росстандарт |
Таджикистан |
TJ |
Таджикстандарт |
Узбекистан |
UZ |
Узстандарт |
4 Приказом Федерального агентства по техническому регулированию и метрологии от 16 ноября 2018 г. N 1023-ст межгосударственный стандарт ГОСТ 34480-2018 введен в действие в качестве национального стандарта Российской Федерации с 1 октября 2019 г.
5 ВВЕДЕН ВПЕРВЫЕ
Информация об изменениях к настоящему стандарту публикуется в ежегодном информационном указателе "Национальные стандарты", а текст изменений и поправок - в ежемесячном информационном указателе "Национальные стандарты". В случае пересмотра (замены) или отмены настоящего стандарта соответствующее уведомление будет опубликовано в ежемесячном информационном указателе "Национальные стандарты". Соответствующая информация, уведомление и тексты размещаются также в информационной системе общего пользования - на официальном сайте Федерального агентства по техническому регулированию и метрологии в сети Интернет (www.gost.ru)
1 Область применения
Настоящий стандарт распространяется на продукты убоя и мясную продукцию, а также на мясо птицы, субпродукты и продукты его переработки, и устанавливает метод определения содержания амфениколов
(хлорамфеникол, флорфеникол, флорфеникол амин, тиамфеникол) и пенициллинов (бензилпенициллин, ампициллин, диклоксациллин, оксациллин, феноксиметилпенициллин, клоксациллин, амоксициллин, нафциллин) с помощью высокоэффективной жидкостной хроматографии с масс-спектрометрическим детектором (ВЭЖХ-МС/МС).
________________
Настоящий стандарт не исключает возможность определения амфениколов и пенициллинов по ГОСТ Р 54904-2012 "Продукты пищевые, продовольственное сырье. Метод определения остаточного содержания сульфаниламидов, нитроимидазолов, пенициллинов, амфениколов с помощью высокоэффективной жидкостной хроматографии с масс-спектрометрическим детектором".
Диапазон измерений для хлорамфеникола - от 0,2 до 1000 мкг/кг, для остальных амфениколов и пенициллинов - от 1,0 до 1000,0 мкг/кг
2 Нормативные ссылки
В настоящем стандарте использованы нормативные ссылки на следующие межгосударственные стандарты:
ГОСТ 12.1.004-91 Система стандартов безопасности труда. Пожарная безопасность. Общие требования
ГОСТ 12.1.007-76 Система стандартов безопасности труда. Вредные вещества. Классификация и общие требования безопасности
ГОСТ 12.1.019-79 Система стандартов безопасности труда. Электробезопасность. Общие требования и номенклатура видов защиты
________________
В Российской Федерации действует ГОСТ Р 12.1.019-2009 "Система стандартов безопасности труда. Электробезопасность. Общие требования и номенклатура видов защиты".
ГОСТ 12.4.009-83 Система стандартов безопасности труда. Пожарная техника для защиты объектов. Основные виды. Размещение и обслуживание
ГОСТ OIML R 76-1-2011 Государственная система обеспечения единства измерений. Весы неавтоматического действия. Часть 1. Метрологические и технические требования. Испытания
ГОСТ 1770-74 (ИСО 1042-83, ИСО 4788-80) Посуда мерная лабораторная стеклянная. Цилиндры, мензурки, колбы, пробирки. Общие технические условия
ГОСТ ISO 3696-2013 Вода для лабораторного анализа. Технические требования и методы контроля
________________
В Российской Федерации действует ГОСТ Р 52501-2005 (ИСО 3696:1987) "Вода для лабораторного анализа. Технические условия".
ГОСТ 4025-95 Мясорубки бытовые. Технические условия
ГОСТ ИСО 5725-2-2002 Точность (правильность и прецизионность) методов и результатов измерений. Часть 2. Основной метод определения повторяемости и воспроизводимости стандартного метода измерений
________________
В Российской Федерации действует ГОСТ Р ИСО 5725-2-2002 "Точность (правильность и прецизионность) методов и результатов измерений. Часть 2. Основной метод определения повторяемости и воспроизводимости стандартного метода измерений".
ГОСТ ИСО 5725-6-2002 Точность (правильность и прецизионность) методов и результатов измерений. Часть 6. Использование значений точности на практике
________________
В Российской Федерации действует ГОСТ Р ИСО 5725-6-2002 "Точность (правильность и прецизионность) методов и результатов измерений. Часть 6. Использование значений точности на практике".
ГОСТ 6709-72 Вода дистиллированная. Технические условия
________________
В Российской Федерации действует ГОСТ Р 58144-2018 "Вода дистиллированная. Технические условия".
ГОСТ 7269-2015 Мясо. Методы отбора образцов и органолептические методы определения свежести
ГОСТ 9792-73 Колбасные изделия и продукты из свинины, баранины, говядины и мяса других видов убойных животных и птиц. Правила приемки и методы отбора проб
ГОСТ 20469-95 Электромясорубки бытовые. Технические условия
ГОСТ 25336-82 Посуда и оборудование лабораторные стеклянные. Типы, основные параметры и размеры
ГОСТ 26272-98 Часы электронно-механические кварцевые наручные и карманные. Общие технические условия
ГОСТ 26678-85 Холодильники и морозильники бытовые электрические компрессионные параметрического ряда. Общие технические условия
ГОСТ 28165-89 Приборы и аппараты лабораторные из стекла. Аквадистилляторы. Испарители. Установки ректификационные. Общие технические требования
ГОСТ 29227-91 (ИСО 835-1-81) Посуда лабораторная стеклянная. Пипетки градуированные. Часть 1. Общие требования
ГОСТ 31467-2012 Мясо птицы, субпродукты и полуфабрикаты из мяса птицы. Методы отбора проб и подготовка их к испытаниям
Примечание - При пользовании настоящим стандартом целесообразно проверить действие ссылочных стандартов в информационной системе общего пользования - на официальном сайте Федерального агентства по техническому регулированию и метрологии в сети Интернет или по ежегодному информационному указателю "Национальные стандарты", который опубликован по состоянию на 1 января текущего года, и по выпускам ежемесячного информационного указателя "Национальные стандарты" за текущий год. Если ссылочный стандарт заменен (изменен), то при пользовании настоящим стандартом следует руководствоваться заменяющим (измененным) стандартом. Если ссылочный стандарт отменен без замены, то положение, в котором дана ссылка на него, применяется в части, не затрагивающей эту ссылку.
3 Термины и определения
В настоящем стандарте применены следующие термины с соответствующими определениями:
3.1 супернатант: Жидкость, располагающаяся над твердым слоем (осадком, седиментом) после центрифугирования пробы.
3.2 элюент: Подвижная фаза (растворитель или смесь растворителей).
3.3 аналит: Вещество, определяемое в пробе объекта аналитического контроля.
4 Сущность метода
Метод основан на извлечении амфениколов и пенициллинов ацетонитрилом, очистке и концентрировании полученного экстракта с помощью твердофазной экстракции (ТФЭ) и последующем количественном определении методом ВЭЖХ-МС/МС.
5 Требования безопасности
5.1 При подготовке и проведении измерений необходимо соблюдать требования техники безопасности при работе с химическими реактивами по ГОСТ 12.1.007.
5.2 Помещение, в котором проводят измерения, должно быть оборудовано приточно-вытяжной вентиляцией. Работу необходимо проводить, соблюдая правила личной гигиены и противопожарной безопасности в соответствии с требованиями ГОСТ 12.1.004, и иметь средства пожаротушения по ГОСТ 12.4.009.
5.3 При работе с электроприборами необходимо соблюдать требования безопасности по ГОСТ 12.1.019.
6 Средства измерений, вспомогательное оборудование, материалы и реактивы
Хроматограф жидкостный высокоэффективный, укомплектованный:
- трехквадрупольным масс-спектрометрическим детектором с источником ионизации распылением в электрическом поле (ESI) с диапазоном измерений массы от 2 до 2000 а.е.м.;
- градиентным насосом;
- хроматографической колонкой для ВЭЖХ длиной 50-150 мм и диаметром 2,1-4,6 мм с обращенной фазой С18, размером частиц 1,8-5,0 мкм;
- блоком термостатирования колонок с поддержанием температуры 40°C с точностью ±0,1°C;
- записывающим устройством с компьютерным управлением и автоматической программой обработки хроматографических данных в соответствии с комплектацией хроматографа.
Весы неавтоматического действия по ГОСТ OIML R 76-1 специального или высокого класса точности или весы лабораторные по нормативным документам государства, принявшего стандарт, с пределами допускаемой абсолютной погрешности не более ±1,0 мг
Баня ультразвуковая лабораторная с регулятором времени.
Испаритель роторный по ГОСТ 28165.
Центрифуга лабораторная с центробежным ускорением 4000 g.
Мясорубка бытовая по ГОСТ 4025 или электромясорубка бытовая по ГОСТ 20469.
Холодильник бытовой электрический по ГОСТ 26678.
Часы электронно-механические по ГОСТ 26272.
Банки стеклянные вместимостью 250-500 см
с крышкой.
Пипетки градуированные 1-2-1-0,5, 1-2-1-1, 1-2-1-2, 1-2-1-5, 1-2-1-10 по ГОСТ 29227 с относительной погрешностью дозирования не более ±5% или дозаторы автоматические с переменным объемом дозирования и относительной погрешностью дозирования не более ±1%.
Колба мерная 2-100-2, 2-500-2 по ГОСТ 1770.
Колба круглодонная К-1-50-29/32 ТХС по ГОСТ 25336.
Пробирки центрифужные из полипропилена вместимостью 15 см.
Флаконы - виалы хроматографические из темного стекла вместимостью 2,0 см.
Фильтр мембранный из политетрафторэтилена с диаметром пор 0,45 мкм.
Вода дистиллированная по ГОСТ 6709 или вода для лабораторного анализа по ГОСТ ISO 3696* первой степени очистки.
________________
* Доступ к международным и зарубежным документам, упомянутым в тексте, можно получить, обратившись в Службу поддержки пользователей. - Примечание изготовителя базы данных.
Кислота муравьиная, ос.ч.
Метанол, ос.ч.
Ацетонитрил, ос.ч.
Картриджи ТФЭ на основе обращенно-фазного сорбента С18 с размером диаметра частиц не более 60 мкм.
Стандартные образцы амфениколов (хлорамфеникол, флорфеникол, флорфеникол амин, тиамфеникол) и пенициллинов (бензилпенициллин, ампициллин, диклоксациллин, оксациллин, феноксиметилпенициллин, клоксациллин, амоксициллин, нафциллин) с содержанием основного вещества не менее 95,0%.
Внутренний стандарт амфениколов - хлорамфеникол-Д5 с содержанием основного вещества не менее 99,0%.
Внутренний стандарт пенициллинов - бензилпенициллин-Д7 с содержанием основного вещества не менее 99,0%.
Допускается применение других средств измерений с метрологическими характеристиками и вспомогательного оборудования с техническими характеристиками не хуже, а также материалов и реактивов по качеству не ниже указанных в настоящем стандарте.
7 Отбор и подготовка проб
7.1 Отбор проб проводят по ГОСТ 7269, ГОСТ 31467, ГОСТ 9792.
7.2 Пробу измельчают, дважды пропуская через мясорубку с диаметром отверстий решетки 2-4 мм, и тщательно перемешивают.
7.3 Подготовленную пробу помещают в стеклянную банку вместимостью 250-500 см, закрывают крышкой и хранят при температуре (4±2)°C не более 2 сут.
Допускается хранить подготовленную пробу в замороженном состоянии при температуре не выше минус 18°C не более 30 сут.
8 Подготовка к измерению
8.1 Приготовление растворов
8.1.1 Приготовление растворов внутренних стандартов анализируемых веществ
Для приготовления растворов внутреннего стандарта хлорамфеникола-Д5 и бензилпенициллина-Д7 взвешивают индивидуальный стандартный образец массой, эквивалентной 10,0 мг определяемого компонента (хлорамфеникол-Д5 или бензилпенициллин-Д7), переносят в мерные колбы вместимостью по 100 см. Для приготовления раствора хлорамфеникола-Д5 доводят объем мерной колбы до метки метанолом. Для приготовления раствора бензилпенициллина-Д7 доводят объем мерной колбы до метки деионизованной водой. По 1,0 см раствора хлорамфеникола-Д5 и бензилпенициллина-Д7 переносят в мерные колбы вместимостью по 100 см и доводят объем до метки деионизованной водой. Расчетная концентрация растворов составляет 1000 нг/см.
Примечание - При расчете концентрации градуировочных растворов учитывают содержание основного вещества в реактиве.
Срок хранения растворов при температуре минус 20°С - не более 9 мес.
8.1.2 Приготовление градуировочных растворов
Для определения амфениколов и пенициллинов готовят градуировочные растворы следующих массовых концентраций: 1000,0 нг/см (раствор 1), 500,0 нг/см (раствор 2), 100,0 нг/см (раствор 3), 10,0 нг/см (раствор 4), 1,0 нг/см (раствор 5), 0,2 нг/см (раствор 6 - для хлорамфеникола).
Для приготовления градуировочных растворов сначала готовят основной раствор. Для этого взвешивают индивидуальный стандартный образец массой, эквивалентной 10,0 мг определяемого компонента (амфениколов и пенициллинов), переносят в мерную колбу вместимостью 100 см и доводят объем до метки метанолом (для амфениколов) или деионизованной водой (для пенициллинов).
Для приготовления раствора 1 в мерную колбу вместимостью 100 см переносят 1,0 см основного раствора и доводят объем до метки деионизованной водой.
Примечание - При расчете концентрации градуировочных растворов учитывают содержание основного вещества в реактиве.
Для приготовления раствора 2 в хроматографическую виалу переносят 0,5 см раствора 1 и 0,5 см деионизованной воды.
Для приготовления раствора 3 в хроматографическую виалу переносят 0,1 см раствора 1 и 0,9 см деионизованной воды.
Для приготовления раствора 4 в хроматографическую виалу переносят 0,1 см раствора 3 и 0,9 см деионизованной воды.
Для приготовления раствора 5 в хроматографическую виалу переносят 0,1 см раствора 4 и 0,9 см деионизованной воды.
Для приготовления раствора 6 в хроматографическую виалу переносят 0,2 см раствора 5 и 0,8 см деионизованной воды.
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