Sub-Group

TTPA - Tobacco and Tobacco Products Analytes (formerly Smokeless Tobacco) - 2008

Objectives

  1. To propose and maintain CORESTA Recommended Methods (CRMs) and related documents for the analysis of tobacco and unburned tobacco products.
  2. To organise interlaboratory testing related to Objective 1.
  3. To organise the manufacture of and maintain smokeless tobacco reference products.

The Smokeless Tobacco Sub-Group (STS) was established in November 2008 by recommendation of the CORESTA Scientific Commission (SC). The initial objectives of the STS were:

  1. To create a report on product definition and definitions of terms to support harmonisation of nomenclature.
  2. To perform collaborative studies on main chemical parameters of smokeless products.
  3. To develop CORESTA Recommended methods as agreed by the Scientific Commission.
  4. To develop a technical report on sample handling and sampling procedures.
  5. To define and set standards for the manufacture of reference products and storage requirements for long term stability.

The STS made significant and continued progress towards all its goals. Since its inception, the STS conducted numerous international collaborative studies, published six CORESTA Recommended Methods (CRMs) and two CORESTA Guides, produced four smokeless tobacco reference products and created the Smokeless Tobacco Glossary. The Smokeless Tobacco Glossary was completed in 2010 and is available on the CORESTA website.

In 2012, the first and fourth objectives were merged into a new fourth objective "to maintain the Guideline on product definition and definitions of terms to support harmonisation of nomenclature" intended to maintain the achieved work. In 2015, the Sub-Group's initial third objective "to define and set standards for the manufacture of reference products and storage requirements for long term stability," was considered complete. In June 2016, the Sub-Group's objectives were fully reviewed and amended to better reflect the focus of its activities.

In January 2017, the Sub-Group changed its name to "Tobacco and Tobacco Product Analytes (TTPA)" in order to work on analytes from a wider range of tobacco products in close cooperation with the Sub-Group Smoke Analytes (formerly "Special Analytes"). In line with this change, reference to "smokeless tobacco" was removed from the first objective and "tobacco and tobacco products" clearly indicated.

In June 2018, the TTPA Sub-Group's revised objectives, as listed above, were approved by the Scientific Commission and the Board. 

CORESTA Recommended Methods

One of the ongoing objectives of the TTPA is to develop CRMs for the chemical and physical characterization of Smokeless Tobacco Products (STP). In recent years, the prioritization of CRM development has been driven by tobacco product regulation or proposed regulation. Manufacturers and contract laboratories from numerous European countries, North America, and Asia participated in the development of the CRMs. Due to the high level of international participation, robust levels of repeatability (r) and reproducibility (R) are determined for each CRM. To date, the following CRMs have been developed or updated to include STPs:

  • CRM 36: Determination of Nitrate in Tobacco and Smokeless Tobacco Products by Reduction to Nitrite and Continuous Flow Analysis (fourth edition)
  • CRM 69: Determination of pH in Tobacco and Tobacco Products (second edition)
  • CRM 71: Smokeless Tobacco Products – Sampling
  • CRM 72: Determination of Tobacco Specific Nitrosamines in Tobacco and Tobacco Products by LC-MS/MS (fourth edition)
  • CRM 76: Determination of Moisture Content (Oven Volatiles) of Tobacco and Tobacco Products (second edition)
  • CRM 86: Determination of Select Carbonyls in Tobacco and Tobacco Products by UHPLC-MS/MS
  • CRM 87: Determination of Nicotine in Tobacco Products by GC/MS

The following CRM has been expanded with CRM 79 to include smokeless tobacco products:

  • CRM 73: Determination of Ammonia in Tobacco by Ion Chromatographic Analysis

The following CRMs have been updated to expand the scope to include smokeless tobacco products:

  • CRM 60: Determination of 1,2-Propylene Glycol and Glycerol in Tobacco and Tobacco Products by Gas Chromatography
  • CRM 61: Determination of 1,2-Propylene Glycol, Glycerol and Sorbitol in Tobacco and Tobacco Products by High Performance Liquid Chromatography

The following CRMs have been updated to expand the scope to include smokeless tobacco products and ground cigars:

  • CRM 56: Determination of Water in Tobacco and Tobacco Products by Karl Fischer Method (third edition)
  • CRM 57: Determination of Water in Tobacco and Tobacco Products by Gas Chromatographic Analysis (second edition)
  • CRM 79: Determination of Ammonia in Tobacco and Tobacco Products by Ion Chromatographic Analysis (second edition)
  • CRM 82: Determination of Benzo[a]pyrene in Tobacco Products by GC-MS (fourth edition)

Robust methods for selected trace metals are still being developed through collaborative studies.

CORESTA Reference Products

Another objective of the TTPA is to develop, produce and maintain reference products. The first part of this objective was fulfilled in 2009 when the former STS SG produced the four CORESTA Reference Products (CRPs) listed below:

  • CRP1: Swedish style snus pouch
  • CRP2: American-style loose moist snuff
  • CRP3: American-style loose dry snuff powder
  • CRP4: American-style loose-leaf chewing tobacco

Due to high demand, a second batch of CRPs was manufactured in 2016. The 2016 CRPs were produced in the same style as the 2009 CRPs except the loose-leaf chewing tobacco was produced in a chopped format.

Reference Products are often used to monitor the analytical processes when conducting routine chemical analyses. Specifically, they are frequently used to assess whether the analytical process is in control and may also be used to compare data generated at different laboratories. Four different CRPs were produced in an effort to have products that covered a wide range of product categories. The CRPs are maintained by North Carolina State University in Raleigh, NC USA at -20 °C. The CRPs can be ordered via the NCSU website https://strp.wordpress.ncsu.edu​. More detailed information on the CRPs can be found on the CORESTA website under "Reference Products" in the Information section.

As mentioned above, the Sub-Group is also responsible for monitoring the stability of the CRPs. In order to fulfill this objective, yearly collaborative studies are conducted in which specific product attributes are monitored. These studies include the determination of pH, moisture (oven volatiles), nicotine, and the four TSNAs (N-nitrosonornicotine (NNN), N-nitrosoanatabine (NAT), N-nitrosoanabasine (NAB) and 4-(N-nitrosomethylamino)-1-(3-pyridyl)-1-butanone (NNK)). The following studies have been conducted to assess the stability of the CRPs:

  • CORESTA Reference Products – 2010 Analysis
  • CORESTA Reference Products – 2011 Analysis
  • CORESTA Reference Products – 2012-2013 Analysis
  • CORESTA Reference Products – 2014 Analysis
  • CORESTA Reference Products – 2015 Analysis
  • CORESTA Reference Products – 2016 Analysis

The 2010, 2011, 2012/2013, 2014, 2015 and 2016 study reports are available on the CORESTA website under "Reports". These studies will continue on an annual basis until the CRPs are shown to no longer be suitable for use as reference products.

CORESTA Guides

A laboratory can only produce high quality results if the integrity of samples is maintained. In this respect, the Sub-Group has produced CORESTA Guide No. 11 (Technical Guideline for Sample Handling of Smokeless Tobacco and Smokeless Tobacco Products) to describe the appropriate storage and preparation of tobacco.

As part of the objective to develop and produce the CRPs, CORESTA Guide No. 15 (CORESTA Reference Products Production and Evaluation Requirements) details the production of the 2009 CRPs and will facilitate the production of CRPs in the future.

Both Guides are published on the CORESTA website under "Guides".

Collaborative Studies

In addition to the work described above, the Sub-Group has conducted several other large collaborative studies (all also available on the CORESTA website under "Reports"). These studies include:

  • CORESTA Smokeless Tobacco Sub-Group Working Group 2 - 2009 Collaborative Study Report (July 2010 - updated Jan 2016). This study included the determination of pH, water, nicotine, moisture and TSNAs in nine commercial STPs.
  • Smokeless Tobacco Sub-Group Technical Report CORESTA Reference Products 2010 Analysis (February 2014). This study included the determination of over 40 analytes in the CRPs.
  • Collaborative and Proficiency Studies. These studies included the determination of nitrates, humectants, ammonia, moisture, select trace metals, benzo[a]pyrene and carbonyls in the CRPs and five commercial STPs.
    • Analysis of Moisture Content (Oven Volatiles) of Smokeless Tobacco Products (March 2014)
    • Determination of Ammonia in Tobacco and Smokeless Tobacco Products (Aug 2014)
    • Determination of Nitrate in Smokeless Tobacco Products by Continuous Flow Analysis - 2010 Collaborative and Proficiency Studies (Jan 2015)
    • 2012 Collaborative Study on Humectants (Feb 2015)
    • Proficiency Test Report - The Determination of Arsenic, Beryllium, Cadmium, Chromium, Cobalt, Nickel, Lead, and Selenium in Reference Materials (2014/2015) (Sept 2015)
    • 2017 Metals Proficiency Test (July 2017)
    • 2015 Collaborative Study on Benzo[a]pyrene in Tobacco Products (March 2016)
    • Determination of Nitrite and Nitrate in Smokeless Tobacco Products by Ion Chromatography and Continuous Flow Analysis - 2016 Collaborative Study (July 2017)
    • 2017 Collaborative Study on Benzo[a]pyrene in Tobacco Products (July 2017) - method modifications to improve CRM 82
    • Select Carbonyls in Tobacco and Tobacco Products - 2016/2017 Collaborative Study (January 2018)
    • 2017 Collaborative Study on Ammonia and Benzo[a]pyrene in Tobacco Products (March 2018)
  • 2016 Collaborative Study on Minor Alkaloids in Tobacco Products (February 2017). This study was carried out in conjunction with the CORESTA Routine Analytical Chemistry (RAC) Sub-Group to investigate methodology suitable for the purpose of determining nornicotine and anabasine in tobacco and tobacco products.
  • 2016 Collaborative Study on Nicotine in Tobacco Products (February 2017). This study was also carried out in together with the CORESTA Routine Analytical Chemistry (RAC) Sub-Group in order to investigate methodology suitable for the purpose of determining nicotine in tobacco and tobacco products. This led to the development of CRM 87.

The purpose of these large collaborative studies was to assess method variability in smokeless tobacco analyses and more recently in ground cigars. Few standardised methods existed for use in these studies and the results were used to help prioritise the development of CRMs.

The TTPA (formerly STS) has provided an invaluable forum for the development of standardised analytical methods (CRMs) for the analysis of STPs. Furthermore, the Sub-Group has enabled numerous industry and contract laboratories to participate in large collaborative studies. Participation in such studies is helpful for laboratories achieving and maintaining their ISO 17025 accreditation. Additionally, these studies provide a means for laboratories to assess their performance as compared to their peers and make improvements when their results differ significantly.

Following the renaming of the Sub-Group and the widening of its remit, further collaborative, interlaboratory and proficiency studies are being undertaken to include a wider range of tobacco products:

  • 2017 Collaborative Study on TSNA, pH, and Moisture (Oven Volatiles) (July 2017).  The intent of these studies was to update the scopes of the applicable CORESTA Recommended Methods (CRMs) to include these additional matrices (in this case ground tobacco, cigarette filler, and cigar filler) as the CRMs currently only include smokeless tobacco products.

 

Updated August 2018

 

Technical Documents

Annual Reports