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Standard Guide for Sample Preparation of Cannabis and Hemp Inflorescence for Laboratory Analysis 实验室分析用大麻和大麻花序样品制备的标准指南
发布日期: 2023-01-15
1.1 在本指南中,概述了获得干大麻/大麻花序测试部分样品的基本步骤。 1.2 样品制备取决于许多因素,包括样品的湿度(干燥度)、待测分析物、浓度/量以及测试方法的精度和准确度要求。在这种情况下,干燥的大麻或大麻植物材料需要从具有代表性的样品中进行粒度减小粉碎,其最终分析测试部分由所采用的测试方法确定。当地监管指南通常规定了从散装材料(收获批次)中提取的代表性样品和用于化学分析的测试部分的最终质量(例如<1 g)。 1.3 由于不同的监管要求不同,本指南并不旨在满足每个地方和州的管辖权;当地/州的要求由用户自行决定是否遵守和解释。 1.4 单位- 以国际单位制表示的数值应视为标准。本标准不包括其他测量单位。 1.5 本标准并不旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前建立适当的安全、健康和环境实践,并确定监管限制的适用性。 1.6 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)委员会发布的《国际标准、指南和建议制定原则决定》中确立的国际公认标准化原则制定的。 =====意义和用途====== 5.1 粉碎的样品制备程序影响其他下游过程,如提取和超声处理,最终影响总分析误差(TAE)和测量不确定度。 5.2 可能影响样品制备过程的因素包括防止先前样品的交叉污染(携带)和样品制备之间的清洁程序不充分、样品处理、储存(样品保存)不良以及植物材料的含水量(干燥方法)大于15 % ( 15 ) 含水量高的样品很难完全加工,在提取和进一步加工过程中可能产生较低的分析物(即大麻素)浓度。最后,水活性规范 D8197年 建议干大麻或大麻花或两者的活性(aw)范围(0.55至0.65)。 5.3 有许多不同类型的硬件技术可以解决干大麻或大麻的粉碎问题;然而,设备列表是详尽的,因此超出了本指南的范围。看见 表3 和 表4 ( 16- 18 ) 以总结不同的铣削技术。不同设备之间的区别通常与样品(干燥、纤维状)的类型、质量和尺寸/形状有关,每种设备对样品最有效。 此外,工厂选择可能有经济原因,即测试实验室的样品吞吐量(每天的样品数量)、获得低温和样品质量要求。 5.4 除取样装置外,本指南不包括食品、酊剂、油/浓缩物、饮料等的样品制备,其中样品多样性对其他工作项目提出了重大样品制备挑战。 5.5 用于粉碎目的的样本量受到限制,因为所需的分析测试部分通常比批量样本小500倍,并且并非每个测试实验室都配备有处理大样本量(即大于100 g干燥的大麻花序/大麻)。 5.6 通过将磨碎的大麻/大麻材料通过标准筛(例如,从#18(1000 μm)的最佳粒径由提取效率进一步确定,其中<1 以前曾报道过大麻和大麻的mm。 5.7 从一个粉碎的初级样品制备多个分析样品,并对其进行平行分析,可获得有关相应分析过程(包括样品制备、注射和整合)重复性的信息,并反映初级样品的同质性。 5.8 在粉碎之前,去除水分至关重要。这一步骤可以通过在从冷冻干燥到室温的各种温度下“干燥”,以及真空烘箱干燥和强制空气烘箱干燥来完成。产品中的一些活性化合物对温度敏感,因此,在一次和二次干燥步骤之前的冷冻干燥预计有利于减少质量恶化。 5.9 当真空将大麻植物保持在-40℃以下时,冷冻干燥通常是一种快速方法 °C,保留了高质量的植物化学物质,例如挥发性化合物(萜烯/萜类化合物)和酸性大麻素。 此外,在通过冷冻(–80 例如,°C冷冻室),或通过添加冷冻剂干冰或液态气体(如液氮)。 5.10 低温研磨可能是减小粒径的首选方法,因为大麻/大麻花序具有许多具有挑战性的材料财产(即水分含量、油/树脂含量和纤维度)。在大麻研磨应用中,通常将液氮直接添加到研磨机中以降低研磨热。另一个步骤可以包括将样品放入液体浴或浸没样品组件中,该液体浴或浸入样品组件在将材料送入低温磨机之前预先冷却材料。如果可用,在研磨过程之前和期间对大麻和大麻花序样品进行低温冷却可以是防止研磨过程中热降解的有效方法。较低的温度可实现: 5.10.1 在研磨之前,在大麻/大麻花序中诱导微观断裂,减少研磨所需的能量。 5.10.2 使植物材料变脆,更易于机械研磨。 5.10.3 它可以降低热容(提供给给定质量的材料以产生单位温度变化的热量),并减少改变大麻/大麻花序温度所需的能量,从而提高研磨效率。根据切割区的材料,LCO可实现最低的切割能力 2. 然后是LN 2. 与材料进料流速相关。
1.1 In this guide, the basic steps in obtaining a test portion sample of either dried cannabis/hemp inflorescence are outlined. 1.2 Sample preparation depends on many factors including moisture (dryness) of the sample, the analyte to be measured, the concentrations/amounts, and the test method's precision and accuracy requirements. In this case, dried cannabis or hemp plant material require particle size reduction-comminution from a representative sample of which the final analytical testing portion is determined by the employed testing method. Local regulatory guidelines often dictate both the representative sample that is taken from the bulk material (harvest batch) and the final mass of the test portion (for example <1 g) for chemical analyses. 1.3 This guide will not purport to meet every local and state jurisdiction since different regulatory requirements vary; the local/state requirements are at the discretion of the user to follow and interpret. 1.4 Units— The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard. 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 5.1 The sample preparation procedure for comminution impacts other downstream processes such as extraction and sonication, which ultimately affects the total analytical error (TAE) and measurement uncertainty. 5.2 Factors that may influence the sample preparation process include the prevention of cross-contamination (carryover) from a prior sample and an inadequate cleaning procedure between preparation of samples, poor sample handling, storage (sample preservation), and moisture content (drying methods) of plant material being greater than 15 % ( 15 ) . Samples with high moisture content are hard to process completely and may yield lower analyte (that is, cannabinoid) concentration during extraction and further processing. Lastly, water activity Specification D8197 is recommended, activity (aw) range (0.55 to 0.65) for dry cannabis or hemp flower or both. 5.3 There are many different types of hardware technologies that address the comminution of dried cannabis or hemp; however, the list of devices is exhaustive and thus beyond the scope of this guide. See Table 3 and Table 4 ( 16- 18 ) for a summary of different milling technologies. Distinctions among various pieces of equipment often relate to the type, mass, and size/shape of the sample (dry, fibrous) for which each is most effective. In addition, there may be economic reasons for mill selection, that is, the sample throughput of the testing laboratory (number of samples per day), access to cryogenics, and sample mass requirements. 5.4 In addition to sampling devices, this guide does not include the sample preparation of edibles, tinctures, oils/concentrates, beverages, and so forth in which the sample diversity poses significant sample preparation challenges to be put forward in additional work items. 5.5 The sample size for comminution purposes is limited as the analytical testing portion required is often 500 times smaller than the bulk sample lot and not every testing laboratory is equipped to handle large sample sizes (that is, greater than 100 g of dried cannabis inflorescence/hemp). 5.6 The particle size is determined by passing the milled cannabis/hemp material through standard sieves, for example, starting with #18 (1000 µm) for the optimum particle size is further determined by extraction efficiency, where <1 mm for cannabis and hemp has been previously reported. 5.7 Preparing multiple analytical samples from one comminuted primary sample and their parallel analysis gives information about the repeatability of the corresponding analytical process (including sample preparation, injection, and integration) and reflects on the homogeneity of the primary sample. 5.8 Moisture removal is critical before any comminution. This step can be accomplished by “drying” at various temperatures ranging from freeze drying to ambient room temperature, as well as vacuum oven drying and forced air oven drying. Some of the active compounds in the product are temperature sensitive, and thus, freeze drying before primary and secondary drying steps is expected to be advantageous in reducing quality deterioration. 5.9 Freeze drying is often a fast approach when a vacuum holds the cannabis plant at temperatures below –40 °C, which retains the high-quality phytochemicals, for example, volatile compounds (terpenes/terpenoids) and acidic forms of cannabinoids. In addition, embrittlement is accomplished before comminution by freezing (–80 °C freezer, for example) for a set time period or by adding cryogen dry ice or liquid gases, such as liquid nitrogen. 5.10 Cryogenic milling may be the preferred way of particle size reduction because of the fact that cannabis/hemp inflorescence exhibits many material properties that can be challenging (that is, moisture content, oil/resin content, and fibrosity). In cannabis milling applications, it is common to add liquid nitrogen directly into the mill to reduce the heat of grinding. Another step may include placing the sample into a liquid bath or immersion sample assembly that pre-cools the material in advance of feeding the material into the cryogenic mill. If available, cryogenic cooling of hemp and cannabis inflorescence samples before and during the grinding process can be an efficient way to prevent thermal degradation during grinding. Lower temperatures may achieve: 5.10.1 Induces microscopic fractures in hemp/cannabis inflorescence before grinding, reducing the energy required to grind it. 5.10.2 Makes the plant material brittle, which is easier to grind mechanically. 5.10.3 It can lower the heat capacity (the amount of heat supplied to a given mass of material to generate a change of unit temperature) and decrease the amount of energy needed to change the temperature of the hemp/cannabis inflorescence, which increases the efficiency of grinding. Depending on the material of the cutting zone, the lowest cutting capability may be achieved with LCO 2 followed by LN 2 correlated to the material feed flow rate.
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归口单位: D37.03
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